CN113249032B - Hydrophobic silica sol precursor composition and preparation method thereof - Google Patents
Hydrophobic silica sol precursor composition and preparation method thereof Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 63
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 35
- 239000002243 precursor Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000077 silane Inorganic materials 0.000 claims abstract description 20
- -1 alkylbenzene sulfonate Chemical class 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 10
- 150000007530 organic bases Chemical class 0.000 claims abstract description 10
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 7
- 125000005375 organosiloxane group Chemical group 0.000 claims abstract description 7
- 229920000570 polyether Polymers 0.000 claims abstract description 7
- XLUBVTJUEUUZMR-UHFFFAOYSA-B silicon(4+);tetraphosphate Chemical compound [Si+4].[Si+4].[Si+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XLUBVTJUEUUZMR-UHFFFAOYSA-B 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 238000003756 stirring Methods 0.000 claims description 23
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 16
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 14
- 239000005871 repellent Substances 0.000 claims description 14
- 230000002940 repellent Effects 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 5
- 229940077388 benzenesulfonate Drugs 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229940035429 isobutyl alcohol Drugs 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 4
- 238000009435 building construction Methods 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 239000004568 cement Substances 0.000 claims description 2
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 claims description 2
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 claims description 2
- WZXYXXWJPMLRGG-UHFFFAOYSA-N hexadecyl benzenesulfonate Chemical compound CCCCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 WZXYXXWJPMLRGG-UHFFFAOYSA-N 0.000 claims description 2
- FFQLQBKXOPDGSG-UHFFFAOYSA-N octadecyl benzenesulfonate Chemical compound CCCCCCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 FFQLQBKXOPDGSG-UHFFFAOYSA-N 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229910052700 potassium Chemical group 0.000 claims description 2
- 239000011591 potassium Chemical group 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- OQNGNXKLDCKIIH-UHFFFAOYSA-N tetradecyl benzenesulfonate Chemical compound CCCCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 OQNGNXKLDCKIIH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 239000010438 granite Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004078 waterproofing Methods 0.000 description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001289 polyvinyl ether Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
- FXSGDOZPBLGOIN-UHFFFAOYSA-N trihydroxy(methoxy)silane Chemical compound CO[Si](O)(O)O FXSGDOZPBLGOIN-UHFFFAOYSA-N 0.000 description 1
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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
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/495—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as oligomers or polymers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/82—Coating or impregnation with organic materials
- C04B41/84—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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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
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- C09D183/14—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 in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
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- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention relates to a hydrophobic silica sol precursor composition and a preparation method thereof. The composition comprises the following components: 5-10 parts of monofunctional silane component A, 30-50 parts of bifunctional silane component B, 5-10 parts of silane coupling agent C, 10-20 parts of solvent D, 5-15 parts of organic base E, 10-20 parts of inorganic base F, 0.4-0.6 part of organosiloxane polyether G, 0.1-0.3 part of long-chain alkylbenzene sulfonate H, 0.1-0.3 part of organic silicon phosphate I and 10-40 parts of water glass J. The hydrophobic silica sol precursor composition prepared according to the invention and the waterproof agent prepared by the hydrophobic silica sol precursor composition improve hydrophobicity and ensure sufficient waterproofness of the material.
Description
Technical Field
The invention relates to a hydrophobic silica sol precursor composition, in particular to a hydrophobic silica sol precursor composition and a preparation method thereof.
Background
The absorption of water and other harmful substances is one of the main factors of various pathological changes of buildings and even the structural or functional damage, so that the waterproof engineering becomes an indispensable process for building construction. The present commonly used building waterproof material is mainly methyl silicate aqueous solution, which is popular because of the advantages of safety, environmental protection, economy, etc. Especially, the method occupies a great position in the field of stone protection.
Along with the development of economic society, the living standard of people is improved, the requirement on building structures is higher and higher, and the traditional methyl silicate material is more and more difficult to meet the application requirement. This is mainly due to the fact that the material only contains methyl groups as hydrophobic groups, and is too basic, and the hydrophobicity and weather resistance are insufficient, and many applications are limited. From the viewpoint of the preparation method, the methylsilicate is prepared by dissolving methylsilicic acid in a strong base. Because the solid is difficult to dissolve, the production cycle is long, the process needs continuous high-temperature heating, the energy consumption is high, the production efficiency is low, and the current concept of energy conservation, environmental protection and greenness is not met.
Although the presence of the oily water repellent overcomes the above problems, the application is still greatly limited due to its high cost and non-compliance with the current stream of safety and environmental protection. Therefore, development of a novel high-performance water-based waterproof material is urgently needed to meet market demand.
Silica sol (hereinafter referred to as silica sol) is used as a novel functional material, belongs to an inorganic material, has excellent weather resistance, has extremely strong surface activity due to the nanometer effect, and is widely applied to preparation of functional composite coatings after modification. Silica sol is generally prepared by hydrolyzing silicate under alkalescent conditions, the sol has strong hydrophilicity, and when the silica sol is applied to water prevention, hydrophobic groups such as long-chain alkyl groups need to be modified on the surface, so that the silica sol with hydrophobicity is obtained.
However, the sol type product obtained directly by the above method has a short shelf life due to the thermodynamic instability of the sol itself and the reduced stability after modification, and is difficult to be commercialized. On the other hand, the preparation process is complex, has accurate requirements on reaction conditions, water quality, pH value and the like, and is not beneficial to large-scale production. More importantly, practice shows that the hydrophobic modified silica sol is directly used as a waterproof agent, although the hydrophobic property is excellent, the film formation is not compact enough, so that the waterproof property is insufficient, and the requirement of building waterproof can not be met.
Disclosure of Invention
[ problem ] to
Therefore, the invention aims to provide a hydrophobic silica sol building waterproofing agent.
It is another object of the present invention to provide a method for preparing the composition.
[ solution ]
According to one embodiment of the present invention, there is provided a hydrophobic silica sol precursor composition comprising:
5 to 10 parts by weight of a monofunctional silane component A,
30 to 50 parts by weight of a bifunctional silane component B,
5 to 10 parts by weight of a silane coupling agent C,
10 to 20 parts by weight of a solvent D,
5 to 15 parts by weight of an organic base E,
10 to 20 parts by weight of an inorganic base F,
0.4 to 0.6 part by weight of an organosiloxane polyether G,
0.1 to 0.3 part by weight of a long-chain alkylbenzene sulfonate H,
0.1 to 0.3 part of organic silicon phosphate I,
10 to 40 parts of water glass J,
wherein the component A is hexamethyldisiloxane or hexamethyldisilazane,
the component B is selected from one or more of dimethyldiethoxysilane, dimethyldimethoxysilane and hydroxyl silicone oil (the viscosity is below 1000 cp),
the component C is one or more selected from KH550, KH790, KH792 and KH560,
the component D is one or more selected from n-butanol, isobutanol, ethylene glycol ethyl ether, ethylene glycol methyl ether and ethylene glycol butyl ether,
the component E is selected from one or more of triethanolamine, diethanolamine and monoethanolamine,
the component F is selected from one or more of sodium hydroxide and potassium hydroxide,
the component G is selected from one or more of organic siloxane polyoxyethylene ether and organic siloxane polyoxypropylene ether,
the component H is selected from one or more of dodecyl benzene sulfonate, tetradecyl benzene sulfonate, hexadecyl benzene sulfonate and octadecyl benzene sulfonate,
the component I is one or more selected from dimethyl phosphate propyl trimethoxy silane, diethyl phosphate propyl trimethoxy silane, dimethyl phosphate propyl sodium silanol and diethyl phosphate propyl potassium silanol
The component J has a structural general formula nM2O.SiO 2, wherein n is 1-4, and M is sodium or potassium.
Preferably, the composition comprises:
6 to 8 parts by weight of a monofunctional silane component A,
34-45 parts by weight of bifunctional silane component B,
6 to 8 parts by weight of a silane coupling agent C,
12 to 15 parts by weight of a solvent D,
8 to 12 parts by weight of an organic base E,
13 to 17 parts by weight of an inorganic base F,
0.4 to 0.6 part by weight of an organosiloxane polyether G,
0.1 to 0.3 part by weight of a long-chain alkylbenzene sulfonate H,
0.1 to 0.3 part of organic silicon phosphate I,
20 to 30 parts of water glass J,
the component D is selected from one or more of n-butyl alcohol, isobutyl alcohol and ethylene glycol butyl ether,
the component E is triethanolamine and is a mixture of triethanolamine,
the component G is organic siloxane polyoxyethylene ether.
According to another embodiment of the present invention, there is provided a method of making a hydrophobic silica sol precursor composition, the method comprising:
a) refluxing and mixing 5-10 parts by weight of monofunctional silane component A, 30-50 parts by weight of bifunctional silane component B, 5-10 parts by weight of silane coupling agent C, 10-20 parts by weight of solvent D and 5-15 parts by weight of organic base E at 60-70 ℃ to obtain mixed solution X,
b) adding 10-20 parts by weight of inorganic base F into 20-30 parts by weight of water, uniformly stirring to obtain alkali liquor Y,
c) keeping the temperature at 60-70 ℃ for reflux, adding the alkali liquor Y into the mixed liquor X under stirring, collecting the fractionated small molecular solvent after the addition is finished, heating to 90-100 ℃ for reflux for 0.5h to obtain colorless viscous liquid Z,
d) adding 10-40 parts of water glass J into 10-20 parts of water by weight, mixing to obtain a mixed solution W,
e) slowly dripping the mixed solution W into the liquid Z at the temperature of about 90 ℃ under stirring, uniformly stirring to obtain a mixture V,
f) when the mixture V in e) is cooled to below 40 ℃, dissolving 0.4-0.6 part by weight of organic siloxane polyether G, 0.1-0.3 part by weight of long-chain alkyl benzene sulfonate H and 0.1-0.3 part by weight of organic silicon phosphate I in 1 part of water, adding the mixture V in e) into the mixture V, uniformly stirring, filtering, and cooling to room temperature to obtain the hydrophobic silica sol precursor composition,
wherein the components A-J are as defined hereinbefore.
Preferably, in the method, the first and second electrodes are,
the component D is selected from one or more of n-butyl alcohol, isobutyl alcohol and ethylene glycol butyl ether,
the component E is triethanolamine and is a mixture of triethanolamine,
the component G is organic siloxane polyoxyethylene ether.
According to another embodiment of the present invention, there is provided a hydrophobic silica sol precursor composition prepared by the above method.
According to another embodiment of the invention, the waterproof agent comprises the hydrophobic silica sol precursor composition and water, wherein the weight ratio of the hydrophobic silica sol precursor composition to the water is 1 (30-100).
According to another embodiment of the present invention, there is provided the use of the hydrophobic silica sol precursor composition described above for a water repellent in building construction.
Preferably, in the application, the hydrophobic silica sol precursor composition is directly coated on the surface of a building such as cement, stone and the like by using water in a ratio of 30-100 times, and then is cured at normal temperature.
Advantageous effects
The hydrophobic silica sol precursor composition provided by the invention is a concentrated product which is prepared at present, realizes water solubility and solves the problem of short storage period. The composition and the further obtained waterproof agent thereof not only improve the hydrophobicity, but also ensure the sufficient waterproofness of the material through the compounding of organic and inorganic components in the formula.
Drawings
FIG. 1 is a photograph of a water repellent (silica sol) according to example 4 of the present invention.
FIG. 2 is a photograph showing the Tyndall phenomenon of the water repellent (silica sol) according to example 4 of the present invention under the action of laser.
FIG. 3 is a photograph showing the effect of lotus leaf water droplets in a water-repellent agent (silica sol) according to example 4 of the present invention applied to granite surface and cured.
Detailed Description
The present invention will be described in more detail in the following examples. However, the following examples are for illustrative purposes only, and the scope of the present invention is not limited thereto.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention unless specifically mentioned. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, regions, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of other features, regions, integers, steps, operations, elements, components, and/or groups thereof.
The starting materials used in the following examples were purchased from Nanjing Neaded chemical Co., Ltd, Guangzhou siloco chemical Co., Ltd, Qingdao Maodde chemical Co., Ltd.
Example 1
Preparation of hydrophobic silica Sol precursor composition 1
a) Uniformly stirring 7 parts by weight of hexamethyldisiloxane (monofunctional silane component A), 40 parts by weight of dimethyldimethoxysilane (bifunctional silane component B), 5 parts by weight of KH550 (silane coupling agent C), 15 parts by weight of isobutanol (solvent D) and 10 parts by weight of triethanolamine (organic base E) in a double-layer reaction kettle with a reflux device, introducing hot oil for heating, and refluxing at 65 ℃ to obtain a mixed solution X1,
b) 15 parts by weight of sodium hydroxide (inorganic base F) was added to 20 parts by weight of water and stirred uniformly to obtain lye Y1,
c) refluxing at 65 deg.C, adding alkali solution Y1 into the mixed solution X1 under stirring, collecting fractionated small molecule solvent, heating to 90 deg.C, refluxing for 0.5h to obtain colorless viscous liquid Z1,
d) 30 parts of sodium water glass (modulus 3) (water glass J) was added to 15 parts by weight of water and mixed to obtain a mixed solution W1,
e) slowly dripping the mixed solution W1 into liquid Z1 at the temperature of about 90 ℃ under stirring, uniformly stirring to obtain a mixture V1,
f) when the mixture V1 in e) is cooled to below 40 ℃, dissolving 0.5 part by weight of organosiloxane polyoxyethylene ether G, 0.2 part by weight of sodium dodecyl benzene sulfonate (long-chain alkyl benzene sulfonate H) and 0.2 part by weight of dimethyl phosphate propyl trimethoxy silane I in 1 part of water, adding the mixture V1 in e), uniformly stirring, filtering, and cooling to room temperature to obtain the hydrophobic silica sol precursor composition.
Example 2
Preparation of hydrophobic silica Sol precursor composition 2
a) 5 parts by weight of hexamethyldisiloxane (monofunctional silane component A), 30 parts by weight of hydroxyl silicone oil (bifunctional silane component B), 5 parts by weight of KH790 (silane coupling agent C), 10 parts by weight of n-butanol (solvent D) and 15 parts by weight of diethanolamine (organic base E) are uniformly stirred in a double-layer reaction kettle with a reflux device, hot oil is introduced for heating, the temperature of the system is kept at 70 ℃ for reflux, and mixed liquor X2 is obtained,
b) 15 parts by weight of potassium hydroxide (inorganic base F) was added to 20 parts by weight of water and stirred uniformly to obtain an alkali solution Y2,
c) refluxing at 70 deg.C, adding alkali solution Y2 into the mixed solution X2 under stirring, collecting fractionated small molecule solvent, heating to 95 deg.C, refluxing for 0.5h to obtain colorless viscous liquid Z2,
d) 15 parts of potassium water glass (modulus 3) (water glass J) was added to 20 parts by weight of water and mixed to obtain a mixed solution W2,
e) slowly dripping the mixed solution W2 into liquid Z2 at the temperature of about 90 ℃ under stirring, uniformly stirring to obtain a mixture V2,
f) when the mixture V2 in e) is cooled to below 40 ℃, dissolving 0.6 part by weight of organosiloxane polypropylene ether G, 0.3 part by weight of sodium dodecyl benzene sulfonate (long-chain alkyl benzene sulfonate H) and 0.2 part by weight of sodium dimethyl phosphate propyl trimethoxy silanol in 1 part of water, adding the mixture into the mixture V2 in e), uniformly stirring, filtering, and cooling to room temperature to obtain the hydrophobic silica sol precursor composition.
Example 3
Preparation of hydrophobic silica Sol precursor composition 3
a) 10 parts by weight of hexamethyldisilazane (monofunctional silane component A), 35 parts by weight of dimethyldiethoxysilane (bifunctional silane component B), 5 parts by weight of KH560 (silane coupling agent C), 10 parts by weight of butyl cellosolve (solvent D) and 15 parts by weight of ethanolamine (organic base E) are uniformly stirred in a double-layer reaction kettle with a reflux device, hot oil is introduced for heating, the temperature of the system is kept at 70 ℃ for reflux, mixed liquor X3 is obtained,
b) 20 parts by weight of potassium hydroxide (inorganic base F) was added to 30 parts by weight of water and stirred uniformly to obtain an alkali solution Y3,
c) refluxing at 70 deg.C, adding alkali solution Y3 into the mixed solution X3 under stirring, collecting fractionated micromolecular solvent, heating to 95 deg.C, refluxing for 0.5h to obtain colorless viscous liquid Z3,
d) 20 parts of sodium water glass (modulus 4) (water glass J) was added to 10 parts by weight of water and mixed to obtain a mixed solution W3,
e) slowly dripping the mixed solution W3 into liquid Z3 at the temperature of about 90 ℃ under stirring, uniformly stirring to obtain a mixture V3,
f) after the mixture V3 in e) is cooled to below 40 ℃, dissolving 0.5 part by weight of organosilicone polyvinyl ether G, 0.3 part by weight of sodium dodecyl benzene sulfonate (long-chain alkyl benzene sulfonate H) and 0.3 part by weight of potassium dimethyl phosphate propyl trimethoxy silanol in 1 part of water, adding the mixture V3 in e) into the mixture V3, uniformly stirring, filtering and cooling to room temperature to obtain the hydrophobic silica sol precursor composition.
Examples 4 to 6
Preparation of water repellent
The compositions 1 to 3 of examples 1 to 3 were mixed and diluted with water at a ratio of 1:30, 1:30 and 1:30, respectively, to give the corresponding water repellent agents 4 to 6.
Experimental examples 7 to 9 compositions and Water repellent Properties test
And (3) stability testing: 500g of each of the compositions 1 to 3 prepared in examples 1 to 3 was placed in a sealed bottle, and stored in a dark place at normal temperature, and after one year, whether or not there was any abnormality such as delamination, precipitation, discoloration, etc. in an observation period, and whether or not the diluted solution was in a sol state was examined by the tyndall phenomenon under a laser beam, and the results were shown in fig. 1 and 2.
Hydrophobicity test: the water repellent prepared in examples 4 to 6 was directly coated on the granite surface, and after curing at normal temperature, the contact angle of a water drop was measured with a contact angle measuring instrument. The granite appearance after curing is seen in fig. 3.
And (3) testing the waterproofness: the water repellent prepared in examples 4 to 6 was directly coated on the surface of granite, and after curing at normal temperature, the water repellency of granite was tested according to JC/T973-2005.
Stain resistance test: the water repellent prepared in examples 4 to 6 was directly coated on the granite surface, and after curing at normal temperature, granite stain resistance was tested according to JC/T973-2005.
Alkali resistance test: the water repellent prepared in examples 4 to 6 was directly coated on the surface of granite, and after curing at normal temperature, the alkali resistance of granite was tested according to JC/T973-2005.
Ultraviolet aging resistance test: the water-proofing agent prepared in examples 4-6 was directly coated on the granite surface, cured at room temperature, and tested for granite ultraviolet aging resistance according to JC/T973-2005.
The results of the above tests and the corresponding dilution factor are listed in table 1 below.
TABLE 1
As can be seen from the results of table 1 above and fig. 1 and 2, the hydrophobic silica sol precursor composition (i.e., the concentrated solution) prepared by the present invention has no problems of delamination, precipitation, discoloration, etc. after being stored for 1 year under the conditions of normal temperature, sealing and light-shielding, has a long storage period, can normally obtain a sol state after dilution, has excellent stability, and is favorable for commercialization.
From the results of table 1 above and fig. 3, it can be seen that the water repellent diluted with the concentrate of the present invention has a contact angle with water of 90 ° or more after curing, has excellent hydrophobicity, and thus can achieve self-cleaning.
The waterproofing agent obtained by diluting the concentrate of the present invention is excellent in waterproofness after curing, and therefore, it can be used for waterproofing of buildings, particularly stone protection.
Claims (8)
1. A hydrophobic silica sol precursor composition, the composition comprising:
5 to 10 parts by weight of a monofunctional silane component A,
30 to 50 parts by weight of a bifunctional silane component B,
5 to 10 parts by weight of a silane coupling agent C,
10 to 20 parts by weight of a solvent D,
5 to 15 parts by weight of an organic base E,
10 to 20 parts by weight of an inorganic base F,
0.4 to 0.6 part by weight of an organosiloxane polyether G,
0.1 to 0.3 part by weight of a long-chain alkylbenzene sulfonate H,
0.1 to 0.3 part of organic silicon phosphate I,
10 to 40 parts of water glass J,
wherein the component A is hexamethyldisiloxane or hexamethyldisilazane,
the component B is selected from one or more of dimethyldiethoxysilane, dimethyldimethoxysilane and hydroxyl silicone oil, and the viscosity of the hydroxyl silicone oil is below 1000 cp;
the component C is selected from one or more of KH550, KH792 and KH560,
the component D is selected from one or more of n-butyl alcohol, isobutyl alcohol, ethylene glycol ethyl ether, ethylene glycol methyl ether and ethylene glycol butyl ether, the component E is selected from one or more of triethanolamine, diethanolamine and monoethanolamine,
the component F is selected from one or more of sodium hydroxide and potassium hydroxide,
the component G is selected from one or more of organic siloxane polyoxyethylene ether and organic siloxane polyoxypropylene ether,
the component H is selected from one or more of dodecyl benzene sulfonate, tetradecyl benzene sulfonate, hexadecyl benzene sulfonate and octadecyl benzene sulfonate,
the component I is one or more of dimethyl phosphate propyl trimethoxy silane, diethyl phosphate propyl trimethoxy silane, dimethyl phosphate propyl sodium silanol and diethyl phosphate propyl potassium silanol
The component J has a structural general formula nM2O.SiO 2, wherein n is 1-4, and M is sodium or potassium.
2. The hydrophobic silica sol precursor composition of claim 1, comprising:
6 to 8 parts by weight of a monofunctional silane component A,
34-45 parts by weight of bifunctional silane component B,
6 to 8 parts by weight of a silane coupling agent C,
12 to 15 parts by weight of a solvent D,
8 to 12 parts by weight of an organic base E,
13 to 17 parts by weight of an inorganic base F,
0.4 to 0.6 part by weight of an organosiloxane polyether G,
0.1 to 0.3 part by weight of a long-chain alkylbenzene sulfonate H,
0.1 to 0.3 part of organic silicon phosphate I,
20 to 30 parts of water glass J,
the component D is selected from one or more of n-butyl alcohol, isobutyl alcohol and ethylene glycol butyl ether,
the component E is triethanolamine and is a mixture of triethanolamine,
the component G is organic siloxane polyoxyethylene ether.
3. A method of making a hydrophobic silica sol precursor composition, the method comprising:
a) refluxing and mixing 5-10 parts by weight of monofunctional silane component A, 30-50 parts by weight of bifunctional silane component B, 5-10 parts by weight of silane coupling agent C, 10-20 parts by weight of solvent D and 5-15 parts by weight of organic base E at 60-70 ℃ to obtain mixed solution X,
b) adding 10-20 parts by weight of inorganic base F into 20-30 parts by weight of water, uniformly stirring to obtain alkali liquor Y,
c) keeping the temperature at 60-70 ℃ for reflux, adding the alkali liquor Y into the mixed liquor X under stirring, collecting the fractionated small molecular solvent after the addition is finished, heating to 90-100 ℃ for reflux for 0.5h to obtain colorless viscous liquid Z,
d) adding 10-40 parts of water glass J into 10-20 parts of water by weight, mixing to obtain a mixed solution W,
e) slowly dripping the mixed solution W into the liquid Z at the temperature of 90 ℃ under stirring, uniformly stirring to obtain a mixture V,
f) when the mixture V in e) is cooled to below 40 ℃, dissolving 0.4-0.6 part by weight of organic siloxane polyether G, 0.1-0.3 part by weight of long-chain alkyl benzene sulfonate H and 0.1-0.3 part by weight of organic silicon phosphate I in 1 part of water, adding the mixture V in e) into the mixture V, uniformly stirring, filtering, and cooling to room temperature to obtain the hydrophobic silica sol precursor composition,
wherein said components A-J are the same as defined in claim 1.
4. The method of claim 3, wherein,
the component D is selected from one or more of n-butyl alcohol, isobutyl alcohol and ethylene glycol butyl ether,
the component E is triethanolamine and is a mixture of triethanolamine,
the component G is organic siloxane polyoxyethylene ether.
5. A hydrophobic silica sol precursor composition prepared by the method of claim 3.
6. A waterproof agent comprising the hydrophobic silica sol precursor composition according to claim 1 and water, wherein the weight ratio of the hydrophobic silica sol precursor composition to the water is 1 (30-100).
7. Use of the hydrophobic silica sol precursor composition according to claim 1 for a water repellent in building construction.
8. The use of claim 7, wherein the hydrophobic silica sol precursor composition is directly coated on the surface of cement and stone buildings by 30-100 times of water, and then is cured at normal temperature.
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