CN116396667B - Green waterproof coating and preparation method thereof - Google Patents
Green waterproof coating and preparation method thereof Download PDFInfo
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- CN116396667B CN116396667B CN202310598097.XA CN202310598097A CN116396667B CN 116396667 B CN116396667 B CN 116396667B CN 202310598097 A CN202310598097 A CN 202310598097A CN 116396667 B CN116396667 B CN 116396667B
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- 238000000576 coating method Methods 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011248 coating agent Substances 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000003822 epoxy resin Substances 0.000 claims abstract description 74
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 74
- 239000008367 deionised water Substances 0.000 claims abstract description 60
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 60
- 239000000839 emulsion Substances 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 36
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 15
- 239000013530 defoamer Substances 0.000 claims abstract description 13
- 229910021352 titanium disilicide Inorganic materials 0.000 claims description 95
- 239000000843 powder Substances 0.000 claims description 79
- DFJQEGUNXWZVAH-UHFFFAOYSA-N bis($l^{2}-silanylidene)titanium Chemical compound [Si]=[Ti]=[Si] DFJQEGUNXWZVAH-UHFFFAOYSA-N 0.000 claims description 75
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical compound FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 claims description 70
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 52
- 239000000243 solution Substances 0.000 claims description 51
- 239000003973 paint Substances 0.000 claims description 45
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 239000012265 solid product Substances 0.000 claims description 24
- -1 divinyl sulfone titanium Chemical compound 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 19
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- AFOSIXZFDONLBT-UHFFFAOYSA-N divinyl sulfone Chemical compound C=CS(=O)(=O)C=C AFOSIXZFDONLBT-UHFFFAOYSA-N 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000004593 Epoxy Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229910021341 titanium silicide Inorganic materials 0.000 claims description 6
- HBJZTQIDFLTRRD-UHFFFAOYSA-M S[Ti] Chemical compound S[Ti] HBJZTQIDFLTRRD-UHFFFAOYSA-M 0.000 claims description 5
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 3
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 239000004848 polyfunctional curative Substances 0.000 description 9
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 150000001336 alkenes Chemical group 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- CGMFKBXPQJJHBR-UHFFFAOYSA-N [SiH3]O[SiH](C=C)C=C Chemical compound [SiH3]O[SiH](C=C)C=C CGMFKBXPQJJHBR-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000008821 health effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000008096 xylene 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/3311—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing a hydroxy group
- C08G65/3312—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing a hydroxy group acyclic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention relates to a green waterproof coating and a preparation method thereof, wherein the green waterproof coating comprises the following two components in parts by weight: the first component comprises: 60-100 parts of aqueous epoxy resin emulsion, 18-30 parts of filler, 0.5-1 part of dispersing agent, 0.3-0.8 part of defoamer, 1.2-2 parts of flatting agent and 20-30 parts of deionized water; the second component comprises: 30-50 parts of aqueous curing agent and 10-20 parts of deionized water; wherein the weight ratio of the first component to the second component is 1:1. The invention discloses a green waterproof coating, which is prepared from aqueous epoxy resin emulsion, and not only solves the defects of poor waterproof property and poor adhesive force commonly existing in the aqueous coating on the market, but also has higher mechanical strength and better heat resistance performance.
Description
Technical Field
The invention relates to the field of green paint, in particular to a green waterproof paint and a preparation method thereof.
Background
Because of the environmental and human health effects of traditional coatings, people now want to develop green coatings, which are energy-saving, low-pollution water-based coatings, powder coatings, high-solid-content coatings (or solvent-free coatings), radiation-curable coatings, and the like. Almost all coatings were solvent borne until the 70 s of the 20 th century. Since the 70 s, more and more low organic solvent content and organic solvent free coatings have been developed due to the increasing price of solvents and the increasingly stringent requirements for reducing VOC emissions.
Along with the increasing perfection of the national environmental protection system and the continuous deep environmental protection consciousness of people, the environmental protection paint is necessarily a trend. The general paint contains strong cancerogenic substances, namely benzene, toluene and xylene, and the decoration can bring pollution to the serious users. But it also contains some other harmful substances, which increasingly hinders the market entry of non-environment-friendly coatings. Solvent-based or oil-based paints have a strong pungent odor and are flammable, explosive, and have inconveniently great consequences once handled carelessly during construction and transportation. And the traditional paint is single and has poor functions. The environment-friendly paint is nontoxic and harmless, does not pollute the environment and does not harm human health.
The green paint is generally water-based or water-emulsion-based material, has no peculiar smell and no combustion, and does not need special requirements for construction and transportation. However, the existing water-based paint has poor waterproof property and insufficient adhesive force, so that the development of the water-based paint is limited.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a green waterproof coating and a preparation method thereof.
The aim of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides a green waterproof coating, which comprises the following two components in parts by weight:
the first component comprises:
60-100 parts of aqueous epoxy resin emulsion, 18-30 parts of filler, 0.5-1 part of dispersing agent, 0.3-0.8 part of defoamer, 1.2-2 parts of flatting agent and 20-30 parts of deionized water;
the second component comprises:
30-50 parts of aqueous curing agent and 10-20 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
Preferably, the configuration process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 60-70 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
step b, adding polyethylene glycol into a reaction bottle, continuously stirring until the mixture is uniform, heating to 80-90 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 5-10 hours to obtain a second mixed solution;
and c, cooling the second mixed solution to 60-70 ℃, continuously adding deionized water, keeping the temperature, stirring for 1-3h, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
Preferably, in the step a, the epoxy resin is bisphenol A type epoxy resin, including E-44 type or E-51 type; the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:4-6.
Preferably, in the step b, the polyethylene glycol comprises one of polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000; the mass ratio of polyethylene glycol to epoxy resin is 1:1-2.
Preferably, in the step b, the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:30-50, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:20-40.
Preferably, in the step c, deionized water is added to the epoxy resin to achieve a solid content of 55% -65%.
Preferably, the dispersant is BYK-180 or BYK-190.
Preferably, the defoamer is an organosilicon defoamer BYK-021 or an organosilicon defoamer BYK-028.
Preferably, the leveling agent is an aqueous leveling agent BYK-333 or an aqueous leveling agent BYK-348.
Preferably, the aqueous epoxy resin is aqueous epoxy hardener WG-528 or aqueous epoxy hardener WG-828, and the manufacturer is Suzhou Mei Guo Wang terrace Material Co.
Preferably, the filler is polymerized coated titanium disilicide, and the preparation method comprises the following steps:
s1, placing titanium disilicide powder into a sodium hydroxide solution, pouring the titanium disilicide powder into a flask after ultrasonic homogenization treatment, stirring the titanium disilicide powder at 40-50 ℃ for 1-3 hours, centrifugally collecting a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 50-60 ℃, stirring for 6-10 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
s3, under the protection of inert gas, dissolving divinyl sulfone into N, N-dimethylformamide, then adding mercapto titanium disilicide powder, dispersing uniformly at room temperature, then adding a photoinitiator, carrying out ultraviolet irradiation reaction for 15-35min, removing solvent and impurities after the reaction is finished, and drying in an oven to obtain the divinyl sulfone titanium disilicide powder;
s4, weighing tetramethyl divinyl disiloxane, dissolving in N, N-dimethylformamide, adding divinyl sulfone titanium disilicide powder, uniformly mixing, adding azo diisobutyronitrile, heating to 60-80 ℃, stirring for reaction for 5-10 hours, centrifugally collecting reaction solid, washing with acetone for three times, and drying in an oven to obtain the polymerized coated titanium disilicide.
Preferably, in the step S1, the particle size of the titanium disilicide powder is 50-100 μm, and the molar concentration of the sodium hydroxide solution is 0.05-0.5mol/L.
Preferably, in the step S1, the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:15-25.
Preferably, in the step S2, the mass ratio of the purified titanium disilicide powder to the 3-mercaptopropyl triethoxysilane to the deionized water is 1:0.15-0.25:10-20.
Preferably, in the step S3, the mass ratio of the titanium mercapto disilicide powder, the divinyl sulfone and the N, N-dimethylformamide is 1:0.36-0.52:10-20.
Preferably, in the step S3, the photoinitiator is benzophenone, and the addition amount is 2.5% -4.5% of the mass of the divinyl sulfone.
Preferably, in the step S4, the mass ratio of the divinyl sulfone titanium disilicide powder, the tetramethyl divinyl disiloxane and the N, N-dimethylformamide is 1.3-2.6:0.5-1:20-30.
Preferably, in the step S4, the addition amount of the azodiisobutyronitrile is 3-7% of the mass of the tetramethyl divinyl disiloxane.
In a second aspect, the present invention provides a method for preparing a green waterproof paint, comprising:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
The beneficial effects of the invention are as follows:
1. the invention discloses a green waterproof coating, which is prepared from aqueous epoxy resin emulsion, and not only solves the defects of poor waterproof property and poor adhesive force commonly existing in the aqueous coating on the market, but also has higher mechanical strength and better heat resistance performance.
2. The invention firstly prepares a water-based epoxy resin emulsion, adopts a chemical modification method, takes bisphenol A epoxy resin as a base, and adds polyethylene glycol into the epoxy resin emulsion so as to introduce hydrophilic hydroxyl groups, so that the hydrophilicity of the epoxy resin is enhanced, and a stable dispersion system can be formed in water. The aqueous epoxy resin emulsion prepared by the method has good water dispersibility, and the compatibility with other additives is also improved, so that the interface performance is better enhanced.
3. The filler in the coating is polymerized coated titanium disilicide, which is prepared by taking titanium disilicide particle powder as a base material and polymerizing and coating the titanium disilicide particle powder on the base material by using tetramethyl divinyl disiloxane and divinyl sulfone. In the preparation process of the polymerized coated titanium disilicide, the titanium disilicide powder is washed by alkali liquor, and the purposes include purification and surface activation; the preparation method comprises the steps of treating and purifying titanium disilicide powder by using a mercapto coupling agent to introduce mercapto groups on the titanium disilicide; the divinyl sulfone is used as a very important ring as a cross-linking agent, so that the whole polymerization reaction is promoted. In the reaction process, one end of the double-end olefin group is firstly combined with mercapto on titanium disilicide in a click reaction way, and then the other end of the double-end olefin group is copolymerized with divinyl disiloxane in a copolymerization way, so that polymerized coated titanium disilicide is formed.
4. The polymerized coating structure of the polymerized coated titanium disilicide prepared by the invention is a high molecular compound, wherein the polymerized coating structure contains thioether groups, sulfonyl groups, organic silicon and various compound groups, and after the polymerized coating structure is compounded with epoxy resin, the polymerized coating structure has stronger bonding property than common inorganic materials, and further improves the properties of the epoxy resin material such as mechanical strength, heat resistance, hydrophobicity, adhesive force and the like.
Detailed Description
The technical features, objects and advantages of the present invention will be more clearly understood from the following detailed description of the technical aspects of the present invention, but should not be construed as limiting the scope of the invention.
Titanium disilicide is used as a material with high strength, high wear resistance and high thermal stability, is widely applied to the ceramic field and the microelectronic field, is used as a filler, and is less, and the titanium disilicide is used as a modified filler in the high-quality coating field by utilizing the characteristics of the titanium disilicide, so that the application range of the titanium disilicide is widened, and more references and references are provided for the development of the high-end coating market.
The invention is further described with reference to the following examples.
Example 1
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
80 parts of aqueous epoxy resin emulsion, 22 parts of polymerized coated titanium disilicide, 0.6 part of dispersant BYK-180, 0.5 part of organosilicon defoamer BYK-021, 1.8 parts of aqueous flatting agent BYK-333 and 25 parts of deionized water;
the second component comprises:
40 parts of aqueous epoxy hardener WG-528 and 15 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
In the first component, the preparation process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing E-44 bisphenol A epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 65 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
wherein the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:5.
Step b, adding polyethylene glycol 4000 into a reaction bottle, continuously stirring until the mixture is uniform, heating to 85 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 8 hours to obtain a second mixed solution;
wherein the mass ratio of polyethylene glycol to epoxy resin is 1:1.5; the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:40, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:30.
And c, cooling the second mixed solution to 65 ℃, continuously adding deionized water, adding the deionized water to the epoxy resin until the solid content reaches 60%, preserving heat and stirring for 2 hours, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
In the first component, the preparation method of the polymerized coated titanium disilicide comprises the following steps:
s1, placing titanium disilicide powder with the particle size of 80 mu m into a 0.2mol/L sodium hydroxide solution, pouring the solution into a flask after ultrasonic homogenization treatment, stirring the solution at 45 ℃ for 2 hours, centrifuging the solution to collect a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
wherein the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:20;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 55 ℃, stirring for 8 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
wherein the mass ratio of the purified titanium disilicide powder to the 3-mercaptopropyl triethoxysilane to the deionized water is 1:0.2:15;
s3, under the protection of inert gas, dissolving divinyl sulfone into N, N-dimethylformamide, then adding mercapto titanium disilicide powder, dispersing uniformly at room temperature, then adding a photoinitiator diphenyl ketone, wherein the addition amount is 3.5% of the mass of the divinyl sulfone, carrying out ultraviolet irradiation reaction for 25min, removing a solvent and impurities after the reaction is finished, and drying in an oven to obtain the divinyl sulfone titanium disilicide powder;
wherein the mass ratio of the titanium mercapto disilicide powder, the divinyl sulfone and the N, N-dimethylformamide is 1:0.45:15;
s4, weighing tetramethyl divinyl disiloxane, dissolving in N, N-dimethylformamide, adding divinyl sulfone titanium disilicide powder, uniformly mixing, then adding azo diisobutyronitrile with the addition amount of 5% of the mass of the tetramethyl divinyl disiloxane, heating to 70 ℃, stirring for reaction for 8 hours, centrifugally collecting reaction solid, washing with acetone for three times, and drying in an oven to obtain polymerized coated titanium disilicide;
wherein the mass ratio of the divinyl sulfone titanium disilicide powder, the tetramethyl divinyl disiloxane and the N, N-dimethylformamide is 1.9:0.7:25.
The preparation method of the green waterproof paint comprises the following steps:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
Example 2
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
60 parts of aqueous epoxy resin emulsion, 18 parts of polymerized coated titanium disilicide, 0.5 part of dispersant BYK-190, 0.3 part of organosilicon defoamer BYK-028, 1.2 parts of aqueous flatting agent BYK-348 and 20 parts of deionized water;
the second component comprises:
30 parts of aqueous epoxy hardener WG-828 and 10 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
In the first component, the preparation process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing E-51 bisphenol A epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 60 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
wherein the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:4.
Step b, adding polyethylene glycol 2000 into a reaction bottle, continuously stirring until the mixture is uniform, heating to 80 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 5 hours to obtain a second mixed solution;
wherein the mass ratio of polyethylene glycol to epoxy resin is 1:1; the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:30, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:20.
And c, cooling the second mixed solution to 60 ℃, continuously adding deionized water, adding the deionized water to the epoxy resin until the solid content reaches 55%, preserving heat and stirring for 1h, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
In the first component, the preparation method of the polymerized coated titanium disilicide comprises the following steps:
s1, placing titanium disilicide powder with the particle size of 50 mu m into a sodium hydroxide solution with the particle size of 0.05mol/L, pouring the titanium disilicide powder into a flask after ultrasonic homogenization treatment, stirring the titanium disilicide powder at the temperature of 40 ℃ for 1h, centrifugally collecting a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
wherein the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:15;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 50 ℃, stirring for 6 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
wherein the mass ratio of the purified titanium disilicide powder to the 3-mercaptopropyl triethoxysilane to the deionized water is 1:0.15:10;
s3, under the protection of inert gas, dissolving divinyl sulfone into N, N-dimethylformamide, then adding mercapto titanium disilicide powder, dispersing uniformly at room temperature, then adding a photoinitiator diphenyl ketone, wherein the addition amount is 2.5% of the mass of the divinyl sulfone, carrying out ultraviolet irradiation reaction for 15min, removing solvent and impurities after the reaction is finished, and drying in an oven to obtain the divinyl sulfone titanium disilicide powder;
wherein the mass ratio of the titanium mercapto disilicide powder, the divinyl sulfone and the N, N-dimethylformamide is 1:0.36:10;
s4, weighing tetramethyl divinyl disiloxane, dissolving in N, N-dimethylformamide, adding divinyl sulfone titanium disilicide powder, uniformly mixing, then adding azo diisobutyronitrile with the addition amount of 3% of the mass of the tetramethyl divinyl disiloxane, heating to 60 ℃, stirring for reaction for 5 hours, centrifugally collecting reaction solid, washing with acetone for three times, and drying in an oven to obtain polymerized coated titanium disilicide;
wherein the mass ratio of the divinyl sulfone titanium disilicide powder, the tetramethyl divinyl disiloxane and the N, N-dimethylformamide is 1.3:0.5:20.
The preparation method of the green waterproof paint comprises the following steps:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
Example 3
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
100 parts of aqueous epoxy resin emulsion, 30 parts of polymerized coated titanium disilicide, 1 part of BYK-180 as a dispersing agent, 0.8 part of an organosilicon defoamer BYK-028, 2 parts of an aqueous leveling agent BYK-333 and 30 parts of deionized water;
the second component comprises:
50 parts of aqueous epoxy hardener WG-828 and 20 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
In the first component, the preparation process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing E-44 bisphenol A epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 70 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
wherein the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:6.
Step b, adding polyethylene glycol 6000 into the reaction bottle, continuously stirring until the mixture is uniform, heating to 90 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 10 hours to obtain a second mixed solution;
wherein the mass ratio of polyethylene glycol to epoxy resin is 1:2; the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:50, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:40.
And c, cooling the second mixed solution to 70 ℃, continuously adding deionized water, adding the deionized water to the epoxy resin until the solid content reaches 65%, preserving heat and stirring for 3 hours, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
In the first component, the preparation method of the polymerized coated titanium disilicide comprises the following steps:
s1, placing titanium disilicide powder with the particle size of 100 mu m into a sodium hydroxide solution with the concentration of 0.5mol/L, pouring the titanium disilicide powder into a flask after ultrasonic homogenization treatment, stirring the titanium disilicide powder at 50 ℃ for 3 hours, centrifugally collecting a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
wherein the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:25;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 60 ℃, stirring for 10 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
wherein the mass ratio of the purified titanium disilicide powder to the 3-mercaptopropyl triethoxysilane to the deionized water is 1:0.25:20;
s3, under the protection of inert gas, dissolving divinyl sulfone into N, N-dimethylformamide, then adding mercapto titanium disilicide powder, dispersing uniformly at room temperature, then adding a photoinitiator diphenyl ketone, wherein the addition amount is 4.5% of the mass of the divinyl sulfone, carrying out ultraviolet irradiation reaction for 35min, removing solvent and impurities after the reaction is finished, and drying in an oven to obtain the divinyl sulfone titanium disilicide powder;
wherein the mass ratio of the titanium mercapto disilicide powder, the divinyl sulfone and the N, N-dimethylformamide is 1:0.52:20;
s4, weighing tetramethyl divinyl disiloxane, dissolving in N, N-dimethylformamide, adding divinyl sulfone titanium disilicide powder, uniformly mixing, then adding azo diisobutyronitrile with the addition amount of 7% of the mass of the tetramethyl divinyl disiloxane, heating to 80 ℃, stirring for reaction for 10 hours, centrifugally collecting reaction solid, washing with acetone for three times, and drying in an oven to obtain polymerized coated titanium disilicide;
wherein the mass ratio of the divinyl sulfone titanium disilicide powder, the tetramethyl divinyl disiloxane and the N, N-dimethylformamide is 2.6:1:30.
The preparation method of the green waterproof paint comprises the following steps:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
Example 4
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
70 parts of aqueous epoxy resin emulsion, 25 parts of polymerized coated titanium disilicide, 0.8 part of dispersant BYK-190, 0.6 part of organosilicon defoamer BYK-028, 1.4 parts of aqueous flatting agent BYK-348 and 22 parts of deionized water;
the second component comprises:
45 parts of aqueous epoxy hardener WG-828 and 16 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
In the first component, the preparation process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing E-51 bisphenol A epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 60 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
wherein the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:5.
Step b, adding polyethylene glycol 2000 into a reaction bottle, continuously stirring until the mixture is uniform, heating to 80 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 10 hours to obtain a second mixed solution;
wherein the mass ratio of polyethylene glycol to epoxy resin is 1:1; the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:50, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:40.
And c, cooling the second mixed solution to 60 ℃, continuously adding deionized water, adding the deionized water to the epoxy resin until the solid content reaches 55%, preserving heat and stirring for 2 hours, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
The preparation method of the polymerization coated titanium disilicide is the same as that of example 1.
The preparation method of the green waterproof paint comprises the following steps:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
Example 5
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
90 parts of aqueous epoxy resin emulsion, 28 parts of polymerized coated titanium disilicide, 0.7 part of dispersant BYK-190, 0.6 part of organosilicon defoamer BYK-028, 1.8 parts of aqueous flatting agent BYK-348 and 28 parts of deionized water;
the second component comprises:
46 parts of aqueous epoxy hardener WG-828 and 14 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
In the first component, the preparation process of the aqueous epoxy resin emulsion comprises the following steps:
step a, mixing E-51 bisphenol A epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 65 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
wherein the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:5.
Step b, adding polyethylene glycol 2000 into a reaction bottle, continuously stirring until the mixture is uniform, heating to 90 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 5 hours to obtain a second mixed solution;
wherein the mass ratio of polyethylene glycol to epoxy resin is 1:2; the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether in a mass ratio of 1:30, and the mass ratio of boron trifluoride diethyl etherate to epoxy resin is 1:20.
And c, cooling the second mixed solution to 60 ℃, continuously adding deionized water, adding the deionized water to the epoxy resin until the solid content reaches 65%, preserving heat and stirring for 3 hours, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
The preparation method of the polymerization coated titanium disilicide is the same as that of example 1.
The preparation method of the green waterproof paint comprises the following steps:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
Comparative example 1
In contrast to example 1, the polymeric coated titanium disilicide was replaced with conventional titanium disilicide.
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
80 parts of aqueous epoxy resin emulsion, 22 parts of titanium disilicide, 0.6 part of dispersant BYK-180, 0.5 part of organosilicon defoamer BYK-021, 1.8 parts of aqueous flatting agent BYK-333 and 25 parts of deionized water;
the second component comprises:
40 parts of aqueous epoxy hardener WG-528 and 15 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
Comparative example 2
In contrast to example 1, the polymeric coated titanium disilicide was replaced with titanium mercapto disilicide powder.
The green waterproof paint comprises the following two components in parts by weight:
the first component comprises:
80 parts of aqueous epoxy resin emulsion, 22 parts of titanium mercapto disilicide powder, 0.6 part of dispersant BYK-180, 0.5 part of organosilicon defoamer BYK-021, 1.8 parts of aqueous flatting agent BYK-333 and 25 parts of deionized water;
the second component comprises:
40 parts of aqueous epoxy hardener WG-528 and 15 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1.
The preparation method of the titanium mercapto disilicide powder comprises the following steps:
s1, placing titanium disilicide powder with the particle size of 80 mu m into a 0.2mol/L sodium hydroxide solution, pouring the solution into a flask after ultrasonic homogenization treatment, stirring the solution at 45 ℃ for 2 hours, centrifuging the solution to collect a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
wherein the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:20;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 55 ℃, stirring for 8 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
wherein the mass ratio of the purified titanium disilicide powder, the 3-mercaptopropyl triethoxysilane and the deionized water is 1:0.2:15.
Experimental example
For the coatings prepared in example 1, examples 4 to 5 and comparative examples 1 to 2, which were coated on steel plates (thickness 125 μm), the coatings were first surface-dried at room temperature, then treated at 120℃for 20 minutes, and after naturally cooling to room temperature, the properties were examined, and some of the reference standards included: GB/T16777-2008 (tensile strength), GB/T9286-1998 (adhesion); GB/T6739-1996 (hardness); GB/T1733-1993 (Water resistance); GB/T1771-1991 (salt spray resistance).
The test results are shown in Table 1:
TABLE 1 detection results for different coatings
| Example 1 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | |
| Tensile Strength (MPa) | 45.6 | 47.2 | 48.5 | 38.1 | 40.3 |
| High temperature resistance (DEG C) | 285 | 283 | 286 | 234 | 252 |
| Adhesion (grade) | 0 | 0 | 0 | 2 | 1 |
| Hardness (Pencil) | 4H | 4H | 5H | 3H | 3H |
| Water resistance (h) | ＞150 | ＞150 | ＞150 | ＜100 | 100-150 |
| Salt spray resistance (h) | ＞500 | ＞500 | ＞500 | ＜300 | 300-500 |
As can be seen from Table 1, the coating prepared by the method of the invention has higher strength, high temperature resistance of more than 280 ℃, adhesion reaching 0 level, hardness higher than 4H, water resistance of more than 150H and salt spray resistance of more than 500H, and the coating prepared by the method of the invention has the advantages of good water resistance, strong adhesion, high strength, high hardness, high temperature resistance and salt spray resistance.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The green waterproof coating is characterized by comprising the following two components in parts by weight:
the first component comprises:
60-100 parts of aqueous epoxy resin emulsion, 18-30 parts of filler, 0.5-1 part of dispersing agent, 0.3-0.8 part of defoamer, 1.2-2 parts of flatting agent and 20-30 parts of deionized water;
the second component comprises:
30-50 parts of aqueous curing agent and 10-20 parts of deionized water;
wherein the weight ratio of the first component to the second component is 1:1;
the filler is polymerized coated titanium disilicide, and the preparation method comprises the following steps:
s1, placing titanium disilicide powder into a sodium hydroxide solution, pouring the titanium disilicide powder into a flask after ultrasonic homogenization treatment, stirring the titanium disilicide powder at 40-50 ℃ for 1-3 hours, centrifugally collecting a solid product, washing the solid product to be neutral by using distilled water, and drying the solid product in an oven to obtain purified titanium disilicide powder;
s2, mixing the purified titanium disilicide powder and 3-mercaptopropyl triethoxysilane in deionized water, heating to 50-60 ℃, stirring for 6-10 hours, centrifugally collecting a solid product, flushing with distilled water for three times, and drying in an oven to obtain the titanium silicide powder;
s3, under the protection of inert gas, dissolving divinyl sulfone into N, N-dimethylformamide, then adding mercapto titanium disilicide powder, dispersing uniformly at room temperature, then adding a photoinitiator, carrying out ultraviolet irradiation reaction for 15-35min, removing solvent and impurities after the reaction is finished, and drying in an oven to obtain the divinyl sulfone titanium disilicide powder;
s4, weighing tetramethyl divinyl disiloxane, dissolving in N, N-dimethylformamide, adding divinyl sulfone titanium disilicide powder, uniformly mixing, adding azo diisobutyronitrile, heating to 60-80 ℃, stirring for reaction for 5-10 hours, centrifugally collecting reaction solid, washing with acetone for three times, and drying in an oven to obtain the polymerized coated titanium disilicide.
2. The green water-proof paint according to claim 1, wherein the configuration process of the aqueous epoxy resin emulsion comprises:
step a, mixing epoxy resin and propylene glycol methyl ether in a reaction bottle, heating to 60-70 ℃, and fully stirring to form a uniform solution to obtain a first mixed solution;
step b, adding polyethylene glycol into a reaction bottle, continuously stirring until the mixture is uniform, heating to 80-90 ℃, dropwise adding boron trifluoride diethyl etherate solution, dropwise adding the boron trifluoride diethyl etherate solution within 1 hour, and stirring at a constant temperature for 5-10 hours to obtain a second mixed solution;
and c, cooling the second mixed solution to 60-70 ℃, continuously adding deionized water, keeping the temperature, stirring for 1-3h, and naturally cooling to normal temperature to obtain the aqueous epoxy resin emulsion.
3. A green water-resistant paint according to claim 2, wherein in the step a, the epoxy resin is bisphenol a type epoxy resin, including E-44 type or E-51 type; the mass ratio of the epoxy resin to the propylene glycol methyl ether is 1:4-6;
in the step b, the polyethylene glycol comprises one of polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000; the mass ratio of polyethylene glycol to epoxy resin is 1:1-2;
in the step b, the boron trifluoride diethyl etherate solution comprises boron trifluoride diethyl etherate and propylene glycol methyl ether with the mass ratio of 1:30-50, and the mass ratio of the boron trifluoride diethyl etherate to the epoxy resin is 1:20-40;
in the step c, deionized water is added to the epoxy resin to achieve the solid content of 55% -65%.
4. A green water-resistant paint according to claim 1, wherein the dispersant is BYK-180 or BYK-190; the defoaming agent is an organosilicon defoaming agent BYK-021 or an organosilicon defoaming agent BYK-028; the leveling agent is a water-based leveling agent BYK-333 or a water-based leveling agent BYK-348; the aqueous curing agent is aqueous epoxy curing agent WG-528 or aqueous epoxy curing agent WG-828.
5. A green waterproof paint according to claim 1, wherein in S1, the particle diameter of the titanium disilicide powder is 50-100 μm, and the molar concentration of the sodium hydroxide solution is 0.05-0.5mol/L; the mass ratio of the titanium disilicide powder to the sodium hydroxide solution is 1:15-25.
6. A green water-proof paint according to claim 1, wherein in S2, the mass ratio of the purified titanium disilicide powder, 3-mercaptopropyl triethoxysilane and deionized water is 1:0.15-0.25:10-20.
7. A green water-proof paint according to claim 1, wherein in S3, the mass ratio of the titanium mercapto disilicide powder, the divinyl sulfone and the N, N-dimethylformamide is 1:0.36-0.52:10-20; the photoinitiator is diphenyl ketone, and the addition amount is 2.5% -4.5% of the mass of the divinyl sulfone.
8. A green water-proof paint according to claim 1, wherein in S4, the mass ratio of the divinyl sulfone titanium disilicide powder, the tetramethyl divinyl disiloxane and the N, N-dimethylformamide is 1.3-2.6:0.5-1:20-30; the addition amount of the azodiisobutyronitrile is 3-7% of the mass of the tetramethyl divinyl disiloxane.
9. A method for preparing the green waterproof paint as claimed in any one of claims 1 to 8, comprising:
(1) Weighing filler, dispersing agent and deionized water in the first component according to the amount, mixing, fully stirring, adding aqueous epoxy resin emulsion, defoaming agent and leveling agent, and fully mixing again to form a first component liquid;
(2) Weighing the aqueous curing agent and deionized water in the second component according to the amount, and fully mixing to form a second component liquid;
(3) When the waterproof paint is required to be used, the first component liquid and the second component liquid are fully mixed, and the green waterproof paint is obtained.
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| CN104558524A (en) * | 2013-10-21 | 2015-04-29 | 北京化工大学 | Preparation method for non-ionic reactive water-borne epoxy resin emulsion |
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| CN115232538A (en) * | 2022-09-02 | 2022-10-25 | 西北永新涂料有限公司 | High-temperature-resistant low-dielectric-loss transformer inner wall heat-conducting insulating water-based anticorrosive paint and preparation method thereof |
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| CN104558524A (en) * | 2013-10-21 | 2015-04-29 | 北京化工大学 | Preparation method for non-ionic reactive water-borne epoxy resin emulsion |
| CN106633078A (en) * | 2016-12-28 | 2017-05-10 | 江苏美思德化学股份有限公司 | Mercapto nano-silica and polyether dual modified organosilicon surfactant and preparation method |
| CN111793434A (en) * | 2020-07-01 | 2020-10-20 | 安徽新大陆特种涂料有限责任公司 | Preparation method of high-temperature-resistant ceramic anticorrosive heat-insulating coating |
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