LU500883B1 - Preparation method of a novel aqueous organic silicon stone protective agent - Google Patents
Preparation method of a novel aqueous organic silicon stone protective agent Download PDFInfo
- Publication number
- LU500883B1 LU500883B1 LU500883A LU500883A LU500883B1 LU 500883 B1 LU500883 B1 LU 500883B1 LU 500883 A LU500883 A LU 500883A LU 500883 A LU500883 A LU 500883A LU 500883 B1 LU500883 B1 LU 500883B1
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- LU
- Luxembourg
- Prior art keywords
- organic silicon
- parts
- protective agent
- stone
- aqueous organic
- Prior art date
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- 239000004575 stone Substances 0.000 title claims abstract description 74
- 239000003223 protective agent Substances 0.000 title claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920001558 organosilicon polymer Polymers 0.000 claims abstract description 27
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 19
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 19
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 150000001343 alkyl silanes Chemical class 0.000 claims description 6
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 claims description 3
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 claims description 3
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 37
- 238000010790 dilution Methods 0.000 abstract description 6
- 239000012895 dilution Substances 0.000 abstract description 6
- 230000035699 permeability Effects 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 5
- 238000004078 waterproofing Methods 0.000 description 5
- 238000005034 decoration Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- GBPOWOIWSYUZMH-UHFFFAOYSA-N sodium;trihydroxy(methyl)silane Chemical compound [Na+].C[Si](O)(O)O GBPOWOIWSYUZMH-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000013517 stratification Methods 0.000 description 2
- 230000002087 whitening effect Effects 0.000 description 2
- RZXLPPRPEOUENN-UHFFFAOYSA-N Chlorfenson Chemical compound C1=CC(Cl)=CC=C1OS(=O)(=O)C1=CC=C(Cl)C=C1 RZXLPPRPEOUENN-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- -1 alum Chemical compound 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000010438 granite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- BDRTVPCFKSUHCJ-UHFFFAOYSA-N molecular hydrogen;potassium Chemical compound [K].[H][H] BDRTVPCFKSUHCJ-UHFFFAOYSA-N 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 239000011814 protection agent Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000007761 roller coating Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
-
- 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
- C04B41/4961—Polyorganosiloxanes, i.e. polymers with a Si-O-Si-O-chain; "silicones"
-
- 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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
A novel of aqueous organic silicon stone protective agent, in parts by weight, the protective agent comprises the following components: self-emulsifying organic silicon polymer solution 50 to 75 parts, silica sol 5 to 10 parts, polyvinyl alcohol 5 to 10 parts 1 to 5 parts of aqueous adhesion promoter. The preparation method is to first prepare a self-emulsifying organic silicon polymer solution by an acid-base two-step method; then add polyvinyl alcohol and silica sol for modification, and finally compound with an accelerator to obtain aqueous organic silicon stone protective agent. The stone protective agent of the present disclosure uses water as a dispersant, has low cost, is safe and non-toxic, has no change in the appearance of the stone after treatment, has good permeability, strong adhesion, fast curing, high dilution ratio, and can be used on the surface and inside of the stone to form protection and comprehensively improve its protection performance.
Description
BL-5325 PREPARATION METHOD OF A NOVEL AQUEOUS ORGANIC SILICON LU500883
[01] The present disclosure relates to the technical field of stone protection, in particular to a novel aqueous organic silicon stone protection agent and a preparation method thereof.
[02] Because of its advantages in decoration and strength, stone is one of the important building materials and has attracted people's attention and favor. Then the porous nature of the stone itself makes the stone susceptible to the influence of the external environment. Under the action of natural factors such as sunlight, weathering and acid rain erosion, it is prone to lesions, decomposition and fragmentation, which seriously affects the beauty and service life of the stone. Therefore, the protection of stone is necessary.
[03] The purpose of the protection is to limit the pollution of the stone and avoid the problems of water spots, stains and chalking during the use of the stone. At present, there are many types of stone protective agents in the market, including inorganic and organic types, as well as solvent-based and aqueous ones. Most of the existing high-end stone protective agents are solvent-based, but there are problems such as high production cost, inconvenience and toxic side effects. Therefore, aqueous is the development direction of stone protective agents.
[04] Methyl silicate is a kind of aqueous organic silicon waterproofing agent. It has long curing time and easy whitening, which affects the coating efficiency and appearance. Publication No. CN101580355 discloses a kind of sodium methylsiliconate as primary raw material. Organic silicon waterproofing agent for building materials, water-proofing agent made of sodium methyl siliconate, silane coupling agent, fatty alcohol polyoxyethylene ether succinate half ester sulfonate, alum, phosphoric acid, polyethylene glycol and water; publication No. CN103571327 discloses a method for preparing stone waterproofing agent by using methyl silicate, silane coupling agent, and polyethylene glycol as raw materials; However, at present, the existing water-based technology products used in stone protection have not overcome the defects of sodium methylsilicate. Therefore, it is still necessary to have the advantages of methyl silicate waterproofing agent in the protection of high-end stone materials to overcome its shortcomings. The present disclosure obtains a product with completely improved performance through self-made organic silicon polymer solution, has a high dilution ratio and does not whiten, and can be applied to high-end stone protection.
[05] The technical problem to be solved by the present disclosure is to provide a aqueous organic silicon stone protective agent and a preparation method thereof in view of the above-mentioned shortcomings of the prior art. In order to form a protective layer on the inside and outside of the stone, the natural appearance of the stone is not affected, 1
BL-5325 and the stone is truly waterproof, weatherproof and stain resistant. LU500883
[06] In order to solve the above-mentioned problems, the technical solutions emoplyed by the present disclosure are as follows:
[07] A novel of aqueous organic silicon stone protective agent. In parts by weight, the protective agent includes the following components: 50-75 parts of self-emulsifying organic silicon polymer solution, 5-10 parts of silica sol, 5-10 parts of polyvinyl alcohol Parts, aqueous adhesion promoter 1-5 parts; the self-emulsifying organic silicon polymer solution is obtained by polymerization of long-chain alkyl silane and amino silane in two steps of acid and alkali, and the solid content is 20-40wt% .
[08] The long-chain alkyl silane is selected from a group consisting of n-butyl triethoxy silane, n-octyl triethoxy silane, and n-dodecyl trimethoxy silane.
[09] The aminosilane is selected from a group consisting of y-aminopropyltriethoxysilane, y-aminopropyltrimethoxysilane, N-(B-aminoethyl)-y-aminopropyltrimethoxysilane, and N--( (Baminoethyl)-y-aminopropylmethyldimethoxysilane.
[10] The silica sol is an alkaline silica sol, with a silica content of 20-30% and a pH value of 9-10.
[11] The average molecular weight of the polyvinyl alcohol is 16,000 to 20,000.
[12] The aqueous adhesion promoter is selected from a group consisting of SA-78, HHG-10, and FZ3667-C.
[13] The preparation method of a novel aqueous organic silicon stone protective agent of the present disclosure comprises the following steps:
[14] (1) Add the long-chain alkyl silane and amino silane to the hydrochloric acid solution at a mass ratio of (5-15):1, stir evenly, heat up to 40-60°C, react for 2-4 hours, and then add potassium hydroxide solid in batch, raise the temperature to 90-100°C, react for 1-2 hours and then lower the temperature to obtain a self-emulsifying organic silicon polymer solution;
[15] (2) In parts by weight, weigh 50-75 parts of the self-emulsifying organic silicon polymer solution prepared in step (1) and 5-10 parts of polyvinyl alcohol, mix and heat to 40-60°C, after the solution is transparent, keep at a constant temperature for 30-60 minutes, lower to room temperature, add 5-10 parts of silica sol and 1-5 parts of aqueous adhesion promoter, stir for 30-60 minutes, and filter to obtain a novel of aqueous organic silicon stone protective agent.
[16] The novel aqueous organic silicon stone protective agent of the present disclosure can be applied to the surface of the stone by brushing, spraying, roller coating or soaking, and penetrates into the micropores or cracks of the stone to form a protective film on the surface and inside of the stone. It overcomes the characteristics of forming a dense protective film on the surface of the stone in the prior art, which causes the micropores of the stone to be blocked, and ensures the air permeability of the stone. Prepared by self-emulsifying organic silicon polymer solution to improve its hydrophobicity and avoid whitening. At the same time, polyvinyl alcohol is added in the modification process to make the hydroxyl group better bond with the stone surface and improve its adhesion. Adhesion promoters shorten the curing time, which is conducive to the improvement of production efficiency. On the one hand, silica sol improves 2
BL-5325 dispersion stability and weather resistance, on the other hand, it also improves adhesion LU500883 and permeability.
[17] Compared with the prior art, the present disclosure has the following beneficial effects: (1) Aqueous environmental protection, non-toxic, non-volatile, non-polluting, and fully meets the requirements of health and environmental protection. (2) The aqueous organic silicon stone protective agent of the present disclosure contains hydrophobic alkyl branched chains, low surface energy silicon-oxygen main chains and polyhydroxyl main chains, thereby ensuring the protective performance and high adhesion of the stone, and ensuring its permeability and stability. (3) Fast curing time, does not change the color of the stone, does not whiten, and maintains the air permeability of the stone. (4) It has a high dilution factor, which can be diluted to 50-80 times. (5) The process is simple, the production efficiency is high, and the cost is low. In summary, the stone protective agent of the present disclosure uses water as a dispersant, has low cost, is safe and non-toxic, has no change in the appearance of the stone after treatment, has good permeability, strong adhesion, fast curing, high dilution ratio, and can Form protection on the surface and inside of the stone, and comprehensively improve its protective performance.
[18] The present disclosure will be described in detail below with reference to specific embodiments. The description in this section is only exemplary and explanatory, and should not have any limitation on the protection scope of the present disclosure.
[19] Example 1
[20] A novel aqueous organic silicon stone protective agent, in parts by weight, including the following components: 75 parts of a self-emulsifying organic silicon polymer solution with a solid content of 20 wt%, 5 parts of silica sol, 5 parts of polyvinyl alcohol, 5 parts of aqueous adhesion promoter .
[21] The preparation method of the novel aqueous organic silicon stone protective agent in this embodiment includes the following steps:
[22] 1) Dissolve 50g methyltriethoxysilane and 10g Y -aminopropyltriethoxysilane in 240g hydrochloric acid solution, stir and dissolve uniformly, heat up to 60°C, react for 2 hours, and then add hydroxide in three batches potassium hydroxide solid, raise the temperature to 90°C, react for 2 hours and then lower the temperature and filter to obtain a 20 wt% self-emulsifying organic silicon polymer solution.
[23] 2) Weigh 75 parts of the self-emulsifying organic silicon polymer solution prepared in step 1) and 5 parts of polyvinyl alcohol, mix and heat to 60°C, wait for the solution to be transparent, keep it at room temperature for 30 minutes, and add 5 parts of silica sol and 5 parts of aqueous adhesion promoter SA-78, stirred for 30 minutes, and filtered to obtain aqueous organic silicon stone protective agent.
[24] Example 2
[25] A novel aqueous organic silicon stone protective agent, in parts by weight, comprising the following components: 50 parts of self-emulsifying organic silicon polymer solution with a solid content of 40 wt%, 10 parts of silica sol, 10 parts of polyvinyl alcohol, 1 part of aqueous adhesion promoter.
3
BL-5325
[26] The preparation method of the novel aqueous organic silicon stone protective LU500883 agent in this embodiment includes the following steps: 271 1) Dissolve 150g of propyltriethoxysilane and 10g of y-aminopropyltrimethoxysilane in 240g of hydrochloric acid solution, stir evenly, heat to 40°C, react for 4 hours, and then add potassium hydroxide solid in four batches , raise the temperature to 90°C, react for 1 hour and then lower the temperature and filter to obtain a 40 wt% self-emulsifying organic silicon polymer solution.
[28] 2) Weigh 50 parts of the 40wt% self-emulsifying organic silicon polymer solution prepared in step 1) and 10 parts of polyvinyl alcohol, mix and heat to 40°C, when the solution is transparent, keep at a constant temperature for 60 minutes, then it is cooled to room temperature, and add 10 parts of silica sol and 1 part of aqueous adhesion promoter FZ3667-C, stir for 60 minutes, filterto obtain aqueous organic silicon stone protective agent.
[29] Example 3
[30] A novel of aqueous organic silicon stone protective agent, in parts by weight, comprising the following components: 60 parts of self-emulsifying organic silicon polymer solution with a solid content of 30 wt%, 8 parts of silica sol, 6 parts of polyvinyl alcohol, 2 parts of aqueous adhesion promoter.
[31] The preparation method of the novel aqueous organic silicon stone protective agent in this embodiment includes the following steps:
[32] 1) Dissolve 100g of n-butyltriethoxysilane = and 10g of N-(B-aminoethyl)-y-aminopropyltrimethoxysilane in 256g of hydrochloric acid solution, stir well, heat up to 50°C, and react for 3 hours, add potassium hydroxide solid in three batches, raise the temperature to 100°C, lower the temperature and filter after 2 hours of reaction to obtain a 30 wt% self-emulsifying organic silicon polymer solution.
[33] 2) Weigh Step 1) Prepare 60 parts of 30wt% self-emulsifying organic silicon polymer solution and 6 parts of polyvinyl alcohol, mix and heat to 50°C, wait for the solution to be transparent, keep it at room temperature for 45 minutes, and add 8 parts of silica sol and 2 parts of aqueous adhesion promoter HHG-10, stir for 60 minutes, filter to obtain aqueous organic silicon stone protective agent.
[34] Example 4
[35] A novel aqueous organic silicon stone protective agent, in parts by weight, comprising the following components: 70 parts of self-emulsifying organic silicon polymer solution with a solid content of 20wt%, 10 parts of silica sol, 5 parts of polyvinyl alcohol, 4 parts of aqueous adhesion promoter.
[36] The preparation method of the novel aqueous organic silicon stone protective agent in this embodiment includes the following steps:
[37] 1) Dissolve 90g of n-octyltriethoxysilane and 10g of N-( B aminoethyl)- Y -aminopropylmethyldimethoxysilane in 100g of hydrochloric acid solution, stir evenly, and heat up to 60°C, reacting for 4 hours, then adding potassium hydroxide solid in three batches, raising the temperature to 100°C, after reacting for 1 hour, cool and filter to obtain a 20 wt% self-emulsifying organic silicon polymer solution.
[38] 2) Weigh 70 parts of the 20wt% self-emulsifying organic silicon polymer solution prepared in step 1) and 5 parts of polyvinyl alcohol, mix and heat to 40°C, after 4
BL-5325 the solution is transparent, keep at a constant temperature for 60 minutes, then cool to LU500883 room temperature, and add 10 parts of silicon sol and 4 parts of aqueous adhesion promoter FZ3667-C, stir for 60 minutes, filter to obtain aqueous organic silicon stone protective agent.
[39] Example 5
[40] A novel aqueous organic silicon stone protective agent, in parts by weight, comprising the following components: 75 parts of self-emulsifying organic silicon polymer solution with a solid content of 20wt%, 5 parts of silica sol, 5 parts of polyvinyl alcohol, 5 parts of aqueous adhesion promoter.
[41] The preparation method of the novel aqueous organic silicon stone protective agent in this embodiment includes the following steps:
[42] 1) Dissolve 90g of n-dodecyltrimethoxysilane and 10g of y-aminopropyltriethoxysilane in 100g of hydrochloric acid solution, stir evenly, heat up to 50°C, react for 3 hours, and then add potassium hydrogen solid in four batches , heat to 100°C, react for 2 hours, and then cool and filter to obtain a 20 wt% self-emulsifying organic silicon polymer solution.
[43] 2) Weigh 75 parts of the 20wt% self-emulsifying organic silicon polymer solution prepared in step 1) and 5 parts of polyvinyl alcohol, mix and heat to 40°C, after the solution is transparent, keep at a constant temperature for 60 minutes, then cool to room temperature, and add 5 parts of silicon sol and 5 parts of aqueous adhesion promoter FZ3667-C, stir for 60 minutes, filter to obtain aqueous organic silicon stone protective agent.
[44] The novel aqueous organic silicon stone protective agents prepared in Examples 1-5 of the present disclosure were respectively coated on marbles, and their performance indicators were tested in accordance with the JC/T 973-2005 "Natural Stone Protective Agents for Building Decoration" standard. The results are as follows: quality grade 1 2 3 4 5 enn | 10 | Loto | toto | toto | toto | too | tone ; Level 0 | Level0 Level 0 Level 0 Level 0 Level 0 Level 0 Resistance resistance resistance resistance No stratification, Stability floating oil and No stratification, floating oil and sedimentation sedimentation
BL-5325 color
[45] The above test results show that the stone protective agent prepared in this embodiment fully meets the requirements of various performance indicators specified by the superior product in JC/T 973-2005 "Natural stone protective agent for building decoration". In addition, the present disclosure is also tested on different stones such as granite, sandstone, and travertine, and its comprehensive protection effect is excellent, and it meets the specified requirements of superior products. Moreover, the stone protective agent is used in dilution, and the dilution to 50-80 times, all meet the requirements of qualified products.
[46] Although the present disclosure gives a detailed description of the above method, those skilled in the art can make improvements based on the above description, and these technical solutions that do not deviate from the spirit of the present disclosure are all within the protection scope of the present disclosure.
6
Claims (7)
1. A novel aqueous organic silicon stone protective agent, wherein, in parts by weight, the protective agent comprises the following components: 50-75 parts of self-emulsifying organic silicon polymer solution, 5-10 parts of silica sol, 5-10 parts of polyvinyl alcohol, 1-5 parts of aqueous adhesion promoter; the self-emulsifying organic silicon polymer solution is obtained by polymerization of long-chain alkyl silane and amino silane in two steps of acid and alkali, the solid content is 20-40wt%.
2. The novel aqueous organic silicon stone protective agent according to claim 1, wherein the long-chain alkyl silane is selected from a group consisting of methyl triethoxy silane, propyl triethoxy silane, n-butyl triethoxysilane, n-octyltriethoxysilane, and n-dodecyltrimethoxysilane.
3. The novel aqueous organic silicon stone protective agent according to claim 1, wherein the aminosilane is selected from a group consisting of y-aminopropyltriethoxysilane, y-aminopropyltrimethoxysilane, N-(B-aminoethyl)-y-aminopropyltrimethoxysilane and N-(B-aminoethyl)-y-aminopropylmethyldimethoxysilane.
4. The novel aqueous organic silicon stone protective agent according to claim 1, wherein the silica sol is alkaline silica sol with a silica content of 20-30% and a pH value of 9 to 10.
5. The novel aqueous organic silicon stone protective agent according to claim 1, wherein the average molecular weight of the polyvinyl alcohol is 16,000 to 20,000.
6. The novel aqueous organic silicon stone protective agent according to claim 1, wherein the aqueous adhesion promoter is selected from a group consisting of SA-78, HHG-10, and FZ3667-C.
7. A preparation method of the novel aqueous organic silicon stone protective agent, wherein the method comprises the following steps: (1) Add the long-chain alkyl silane and amino silane to the hydrochloric acid solution at a mass ratio of (5-15):1, stir evenly, heat up to 40-60°C, react for 2-4 hours, and then add potassium hydroxide solid in batch, raise the temperature to 90-100°C, react for 1-2 hours and then lower the temperature and filter to obtain a self-emulsifying organic silicon polymer solution; (2) In parts by weight, weigh 50-75 parts of the self-emulsifying organic silicon polymer solution prepared in step (1) and 5-10 parts of polyvinyl alcohol, mix and heat to 40-60°C, when the solution is transparent, keep at a constant temperature for 30-60 minutes, lower to room temperature, add 5-10 parts of silica sol and 1-5 parts of aqueous adhesion promoter, stir for 30-60 minutes, and filter to obtain a novel of aqueous organic silicon stone protective agent.
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