CN116656230B - Preparation method of water-based normal-temperature self-drying organic silicon multi-hybrid resin - Google Patents
Preparation method of water-based normal-temperature self-drying organic silicon multi-hybrid resin Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000011347 resin Substances 0.000 title claims abstract description 27
- 229920005989 resin Polymers 0.000 title claims abstract description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 16
- 239000010703 silicon Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001035 drying Methods 0.000 title claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 19
- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims abstract description 13
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004132 cross linking Methods 0.000 claims abstract description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract 3
- 230000007062 hydrolysis Effects 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 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 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 5
- -1 Diphenyl diethyl siloxane Chemical class 0.000 claims description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 235000010290 biphenyl Nutrition 0.000 claims 1
- 239000004305 biphenyl Substances 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims 1
- ZOSUYJQQKCDDLV-UHFFFAOYSA-N triethyl(methylsilyloxy)silane Chemical compound CC[Si](CC)(CC)O[SiH2]C ZOSUYJQQKCDDLV-UHFFFAOYSA-N 0.000 claims 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000009396 hybridization Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
- 125000005375 organosiloxane group Chemical group 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000003973 paint Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 125000005037 alkyl phenyl group Chemical group 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical group O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
- C08F230/085—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon the monomer being a polymerisable silane, e.g. (meth)acryloyloxy trialkoxy silanes or vinyl trialkoxysilanes
-
- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a preparation method of high-performance water-based normal-temperature self-drying organic silicon multi-component hybrid resin, which belongs to the field of high polymer materials, and the research product is prepared by copolymerizing vinyl triethoxysilane and triethylene glycol dimethacrylate into a linear low-component polymer, and then carrying out co-hydrolysis with methyltriethylsil, phenyl triethylsiloxane and tetraethoxysilane to form the organic-inorganic block-copolymerized multi-component hybrid resin under the condition of modifying silica-alumina sol by a crosslinking catalyst. Preparation and Synthesis principle 1. Copolymerization of vinyltriethoxysilane and triethylene glycol dimethacrylate 2. Hydrolysis of organosiloxanes 3. Condensation hybridization reaction
Description
Technical field: the invention relates to a preparation method of high-performance environment-friendly water-based normal-temperature self-drying organic silicon multi-component hybrid resin, which belongs to the field of chemical building materials and can be applied to the manufacture of finish protection of various water-based coatings, water-based high-temperature-resistant paint, anti-corrosion paint and the like.
The background technology is as follows: the organic silicon resin coating is widely applied to industries such as national defense and military industry, electrical industry, leather industry, light industry products, rubber plastics, food sanitation and the like due to the characteristics of excellent thermal oxidation stability, electrical insulation property, weather resistance, water resistance, salt spray resistance, mould resistance, biocompatibility and the like, but has the defects of poor adhesion to substrates, poor paint film toughness, high price and the like, the application range of the organic silicon resin coating is limited to a certain extent, most of the organic silicon resins in the current market are solvent-based, high-temperature baking and drying are mainly, certain pollution is caused to the environment, the construction environment is required, the adhesion of acrylic resin to various substrates is good, the paint film toughness is good, but the high-temperature resistance is poor, the weather resistance is not as good as organic silicon resin, so that the research on an aqueous normal-temperature self-drying resin organic silicon multi-hybrid resin becomes a necessary, and the organic silicon multi-hybrid resin has more innovative technology in the field at home and abroad, but has the advantages of cost control and complete water-based on the aspects of synthetic technology.
The invention comprises the following steps: the invention aims to prepare a water-based normal-temperature self-drying type organic silicon multi-component hybrid resin, wherein acrylic acid monomer triethylene glycol dimethacrylate is introduced to improve the toughness and the adhesive force of the resin to a base material, pseudo-boehmite is aluminum hydroxide monohydrate, silica sol is mSiO2.nH2O, the surface of SiO2 contains a large amount of water and hydroxyl groups, the silica-alumina sol contains-O-Si-, -O-Al-, the silica-alumina sol is used as a catalyst through modification of KH-560, and simultaneously, the hybridization reaction is introduced to introduce an alumina bond to improve the wear resistance, the water-based property and the self-drying property of the resin.
The purpose of the invention is implemented by the following technical scheme:
1. Preparation of vinyl triethoxysilane, triethylene glycol dimethacrylate Low molecular weight copolymer: 90g of cosolvent isopropanol, 65g of ethylene glycol monobutyl ether, 65g of dipropylene glycol methyl ether, 130g of vinyltriethoxysilane, 6g of azodiisobutyronitrile and 7.8g of n-dodecyl mercaptan are added into a 1000ML four-neck flask provided with a stirring thermometer, a reflux condenser and a dropping funnel, the cosolvent is completely dissolved, the temperature is raised to 95 ℃, 100g of triethylene glycol dimethacrylate and 6g of azodiisobutyronitrile are placed into the dropping funnel, the dropping is completed at a constant speed within 3 hours under the condition of keeping 95 ℃, and 0.3 of azodiisobutyronitrile is added under the stirring state, and the temperature is kept for 2 hours.
2. Preparation of crosslinking catalyst modified silica alumina sol: (1) 100 g of silica sol is placed in a 500ML four-neck flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel, the temperature is raised to 50 ℃ in a water bath kettle, 3ML of gamma-glycidoxypropyl trimethoxy silicon (KH-560) is added dropwise under stirring, and stirring is carried out for 4-6 hours. (2) 250ml deionized water and 5g nitric acid are added into a 500ml beaker, 50 g pseudo-boehmite is slowly added into the beaker under the high-speed stirring state in a high-speed dispersing machine, and the mixture is dispersed for about 1 hour. (3) Adding the step (2) into the step (1), stirring for 2 hours at 50 ℃, and forming Al2O3 sol by pseudo-boehmite in nitric acid solution, wherein the main component is AlOOH, and forming copolycondensation reaction with hydroxyl in silica sol under the action of a coupling agent KH-560 to obtain the crosslinking catalyst modified silica alumina sol with a storage stability period of more than 6 months.
3. Preparation of water-based normal-temperature self-drying organic silicon multi-hybrid resin: a1000 ml four-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a dropping funnel was charged with vinyltriethoxysilane, triethylene glycol dimethacrylate copolymer. And one or more of methyltriethoxysilicon, dimethyldiethoxysilane, phenyltriethylsiloxane and diphenyldiethylsiloxane, deionized water, stirring uniformly and heating to 40 ℃, putting silica-alumina sol into a dropping funnel, dropwise adding the silica-alumina sol within 1 hour, stirring at 40 ℃ for 2 hours until the organosilicon monomer is completely hydrolyzed, heating to 70 ℃ and stirring for 2 hours, heating to 80 ℃ and stirring for 1 hour, cooling to normal temperature, neutralizing with ammonia water and pH value of about 7, and filtering to obtain the transparent bluish-light water-based organosilicon multi-component hybrid resin.
Specific embodiments:
Example 1: 100 g of methyltriethoxysilicon, 60 g of alkylphenyl triethylsiloxane, 45 g of copolymer of vinyltriethoxysilane and triethylene glycol dimethacrylate and 100 g of deionized water are added into a 1000ml four-neck flask provided with a stirrer, a thermometer, a reflux condenser and a dropping funnel, 200 g of silica alumina sol is placed into the dropping funnel, dropwise added is completed within 1 hour, stirred at 40 ℃ for 2 hours until the organosilicon monomer is completely hydrolyzed, then heated to 70 ℃ for 2 hours, then heated to 80 ℃ for stirring for 1 hour, cooled to normal temperature, and the pH value is about 7, and the transparent blue light water-based organosilicon multi-component hybrid resin is obtained by filtering.
Example 2: 100 g of methyltriethoxysilane, 50 g of dimethyldiethoxysilane, 20 g of tetraethoxysilane, 45 g of copolymer of vinyltriethoxysilane and triethylene glycol dimethacrylate, 110 g of deionized water, uniformly stirring and heating to 40 ℃, placing 220 g of silica alumina sol into a dropping funnel, dropwise adding the silica alumina sol within 1 hour, stirring at 40 ℃ for 2 hours until the organosilicon monomer is completely hydrolyzed, heating to 70 ℃ for 2 hours, stirring at 80 ℃ for 1 hour, cooling to normal temperature, neutralizing the PH value with ammonia water to about 7, and filtering to obtain the transparent blue light water-based organosilicon multi-component hybrid resin.
Example 3: 100 g of methyltriethoxysilicon, 60 g of alkylphenyl triethylsiloxane, 20 g of tetraethoxysilane, 45 g of copolymer of vinyltriethoxysilane and triethylene glycol dimethacrylate, 90 g of deionized water, uniformly stirring and heating to 40 ℃, 180 g of silica alumina sol is placed in a dropping funnel, dropwise adding is completed in 1 hour, stirring is carried out at 40 ℃ for 2 hours until the organosilicon monomer is completely hydrolyzed, heating is carried out at 70 ℃ for 2 hours, stirring is carried out at 80 ℃ for 1 hour, cooling is carried out to normal temperature, the pH value is about 7, and the transparent blue light water-based organosilicon multi-component hybrid resin is obtained by filtering.
Performance index of the polybasic hybrid resin:
Appearance: a blue light-carrying transparent liquid;
pH value: 7, preparing a base material;
Solid content: 38%;
Water solubility: the resin is still blue transparent liquid after being diluted with water in any ratio.
The properties of the resins of the examples and the varnishes produced therefrom are shown in the table:
TABLE 1 preparation of test templates
TABLE 2 index detection
Claims (3)
1. The preparation method of the water-based normal-temperature self-drying organic silicon multi-hybrid resin is characterized by comprising the following steps of:
Composition weight
Vinyl triethoxysilane, triethylene glycol dimethacrylate low molecular weight copolymer 40-60
Methyltriethylsiloxysilane 50-150
50-150% Of dimethyldiethoxysilane
Phenyl triethylsiloxane 30-80
Diphenyl diethyl siloxane 30-80
Tetraethoxysilane 10-30
Modified silica alumina sol 120-260
Isopropanol 20-50
80-160 Parts of deionized water
The preparation method comprises the following steps: adding vinyl triethoxysilane, triethylene glycol dimethacrylate low molecular weight copolymer, methyl triethoxysilane, dimethyl diethoxysilane, phenyl triethyl siloxane, diphenyl diethyl siloxane and deionized water into a 1000mL four-neck flask with a stirring thermometer, a reflux condenser and a dropping funnel, uniformly stirring and heating to 40 ℃, putting the modified silica alumina sol into the dropping funnel, dropwise adding the modified silica alumina sol in 1 hour, stirring at 40 ℃ for 2 hours until the organosilicon monomer is completely hydrolyzed, heating to 70 ℃, stirring for 2 hours, heating to 80 ℃ and stirring for 1 hour, and filtering to obtain the viscous transparent blue light water-based organosilicon multi-component hybrid resin;
the preparation of the modified silica-alumina sol comprises the following steps:
The preparation method comprises the following steps: placing 100g of acidic silica sol into a 500mL four-neck flask provided with a stirrer, a thermometer, a reflux condenser and a dropping funnel, heating to 50 ℃ in a water bath kettle, dropwise adding 3mL of gamma-glycidoxypropyl trimethoxysilane in a stirring state, and stirring for 4-6 hours; adding 250mL of deionized water and 5g of nitric acid into a 500mL beaker, slowly adding 50 g of pseudo-boehmite into the beaker under a high-speed stirring state in a high-speed dispersing machine, and dispersing for 1 hour; c, adding the b into the a, and stirring for 30 minutes at 50 ℃ to obtain the crosslinking catalyst modified silica-alumina sol with the storage stability period of more than 6 months.
2. The method for preparing the aqueous normal-temperature self-drying organosilicon multi-hybrid resin according to claim 1, wherein the low molecular weight copolymer of vinyl triethoxysilane and triethylene glycol dimethacrylate
The preparation method comprises the following steps: 90g of cosolvent isopropanol, 65g of ethylene glycol monobutyl ether, 65g of dipropylene glycol methyl ether, 130g of vinyltriethoxysilane, 6g of azobisisobutyronitrile and 7.8g of n-dodecyl mercaptan are added into a 1000mL four-neck flask provided with a stirring thermometer, a reflux condenser and a dropping funnel, the cosolvent is completely dissolved, the temperature is raised to 95 ℃, 100g of triethylene glycol dimethacrylate and 6g of azobisisobutyronitrile are placed into the dropping funnel, the dropping is completed within 3 hours at a constant speed, 0.3g of azobisisobutyronitrile is added under the stirring state, and the temperature is kept for 2 hours.
3. The preparation method of the water-based normal-temperature self-drying organic silicon multi-hybrid resin is characterized in that vinyl triethoxysilane and triethylene glycol dimethacrylate low molecular weight copolymer are organic-inorganic hybrid monomers, modified silica-alumina sol is inorganic hybrid monomers and an organic silicon hydrolysis catalyst, and the organic silicon monomers are methyltriethoxysilicone, dimethyldiethoxysilane, phenyl triethylsiloxane and diphenyl diethylsiloxane.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766403A (en) * | 2012-07-13 | 2012-11-07 | 太仓富勒姆纳米新材料科技有限公司 | Acrylic-modified organosilicon nano paint and preparation method thereof |
| CN115304942A (en) * | 2022-08-16 | 2022-11-08 | 上海保耐舒新材料技术有限公司 | Water-based long-acting antifogging self-cleaning coating and preparation method thereof |
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| CN103146303B (en) * | 2013-03-22 | 2015-04-15 | 南昌航空大学 | Method for preparing high-temperature-resistant anti-corrosion organosilicon/alumina nanometer hybrid coating through supercritical drying |
| CN103937300A (en) * | 2014-04-22 | 2014-07-23 | 浙江倍斯特制冷科技有限公司 | Anticorrosion treatment method for cooling tower metal parts and coating used in anticorrosion treatment method |
| CN106800394A (en) * | 2016-12-19 | 2017-06-06 | 马鞍山杰创塑胶科技有限公司 | A kind of silica sol modified regeneration EPS nanoparticulate silicates cementitious composite foaming insulation boards of hydridization and preparation method thereof |
| CN106833244B (en) * | 2017-01-11 | 2019-06-18 | 华南理工大学 | Mono-component organic silicone oxygen alkane/inorganic silica solution hydridization high silicon content polyacrylate water-borne dispersions and preparation method thereof |
| KR20190008606A (en) * | 2017-07-17 | 2019-01-25 | 정덕교 | Expansible organic-inorganic hybrid grouting solution and method for construction using the same |
| CN108546485B (en) * | 2017-12-04 | 2021-01-12 | 苏州吉人高新材料股份有限公司 | High-solid-content organic-inorganic hybrid resin and preparation method thereof |
| CN109504280B (en) * | 2018-11-29 | 2020-09-29 | 安徽工业大学 | Preparation method of silicon-aluminum composite sol coating on surface of magnesium alloy |
| CN110003383B (en) * | 2019-04-03 | 2021-02-02 | 广州五行材料科技有限公司 | Silicon-titanium hybrid acrylate polymer and dual-curing coating prepared from same |
| CN112358617B (en) * | 2020-09-23 | 2022-08-23 | 中昊北方涂料工业研究设计院有限公司 | Composite organic silicon resin and high-temperature-resistant coating |
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| CN115304942A (en) * | 2022-08-16 | 2022-11-08 | 上海保耐舒新材料技术有限公司 | Water-based long-acting antifogging self-cleaning coating and preparation method thereof |
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