CN116254085A - Weather-resistant MS door and window glue and preparation method thereof - Google Patents
Weather-resistant MS door and window glue and preparation method thereof Download PDFInfo
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- CN116254085A CN116254085A CN202310115025.5A CN202310115025A CN116254085A CN 116254085 A CN116254085 A CN 116254085A CN 202310115025 A CN202310115025 A CN 202310115025A CN 116254085 A CN116254085 A CN 116254085A
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- 239000003292 glue Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 14
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 72
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 36
- 229920000642 polymer Polymers 0.000 claims abstract description 31
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 239000003381 stabilizer Substances 0.000 claims abstract description 18
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 13
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000012965 benzophenone Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims description 23
- 239000011347 resin Substances 0.000 claims description 23
- 239000000853 adhesive Substances 0.000 claims description 14
- 230000001070 adhesive effect Effects 0.000 claims description 14
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical class [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 230000003712 anti-aging effect Effects 0.000 claims description 8
- 230000004224 protection Effects 0.000 claims description 8
- -1 Stearic acid modified calcium Chemical class 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical group CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- XYYQWMDBQFSCPB-UHFFFAOYSA-N dimethoxymethylsilane Chemical compound COC([SiH3])OC XYYQWMDBQFSCPB-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 230000032683 aging Effects 0.000 abstract description 13
- 230000004580 weight loss Effects 0.000 abstract description 6
- 230000006750 UV protection Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000013329 compounding Methods 0.000 abstract 1
- 239000000565 sealant Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000003860 storage Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NPFYZDNDJHZQKY-UHFFFAOYSA-N 4-Hydroxybenzophenone Chemical compound C1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 NPFYZDNDJHZQKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000011345 viscous material Substances 0.000 description 2
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- LGDOCZGADCEJIG-UHFFFAOYSA-N ethane;trimethoxysilicon Chemical compound CC.CO[Si](OC)OC LGDOCZGADCEJIG-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 238000005303 weighing Methods 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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides weather-resistant MS door and window glue and a preparation method thereof. The weather-resistant MS door and window glue is prepared by compounding MS polymer, benzophenone modified oligomeric silsesquioxane, calcium carbonate, polypropylene glycol, auxiliary agent, stabilizer, silane coupling agent and catalyst according to a specific proportion. MS door and window glue containing the modified oligomeric silsesquioxane completely meets the standard requirement of GB/T14683 in the building industry, and has the advantages of low thermal weight loss and capability of effectively improving the water ultraviolet resistance and the wet heat aging resistance.
Description
Technical Field
The invention relates to the technical field of building adhesives, in particular to weather-resistant MS door and window adhesive and a preparation method thereof.
Background
The building door and window glue is used for sealing joints between a window frame and glass and joints between the window frame and an inner wall body and an outer wall body, and plays a vital role in the aspects of air tightness, waterproofness, heat preservation, sound insulation and the like of doors and windows. Building door and window glue needs to withstand weather such as wind, sun, rain and the like all the year round, and when the sealant is continuously aged, once the sealant fails, the problems of water leakage, air leakage and the like can be generated, so that the house quality and the use feeling are seriously affected.
At present, silicone door and window adhesives are mainly used in the market, but with price competition, products are good and bad, the service life of the door and window adhesives is reduced because of cost reduction caused by adding mineral oil such as white oil instead of silicone oil, and the continuous volatilization of the white oil causes door and window and environmental pollution. Therefore, the development of the weather-proof MS door and window glue has great use value and environmental protection significance.
Disclosure of Invention
Based on the above, it is necessary to provide a weather-proof MS door and window glue and a preparation method thereof, which are not only suitable for bonding, sealing and waterproofing of window frames, glass and inner and outer walls, but also have lower thermal weightlessness performance and better water ultraviolet resistance and humid heat aging performance.
The invention adopts the following technical scheme:
the invention provides weather-resistant MS door and window glue which is mainly prepared from the following raw materials in parts by weight: 100 parts of MS polymer, 20-40 parts of benzophenone modified oligomeric silsesquioxane, 200-400 parts of calcium carbonate, 80-120 parts of polypropylene glycol, 2-5 parts of anti-aging auxiliary agent, 10-20 parts of stabilizer, 5-9 parts of silane coupling agent and 0.3-1 part of catalyst;
wherein the MS polymer is selected from the following components in percentage by weight (1-3): 1 and trimethoxystp type polymer.
The dimethoxymethylsilyl polyether type polymer has the structural formula:
the trimethoxySTP type polymer has the structural formula:
the diphenyl ketone modified oligomeric silsesquioxane has the structural formula:
preferably, the MS polymer is selected from the group consisting of (1 to 2.5) by weight: 1 and trimethoxystp type polymer.
Preferably, the weather-proof MS door and window glue is prepared from the following raw materials in parts by weight: 100 parts of MS polymer, 30 parts of benzophenone modified oligomeric silsesquioxane, 280 parts of calcium carbonate, 90 parts of polypropylene glycol, 4 parts of anti-aging auxiliary agent, 15 parts of stabilizer, 7 parts of silane coupling agent and 0.6 part of catalyst.
Preferably, the dimethoxymethylsilane-based polyether polymer is selected from the group consisting of S810 resins having an average viscosity at 25℃of 18-23 Pa.s.
Preferably, the trimethoxySTP polymer 3368T resin and 30000T resin have an average viscosity of 30-40 Pa.s at 25 ℃.
The MS polymer adopts the method of using the two resins in a matching way, so that the product has the advantages of fast deep solidification and long operability; in addition, the preparation process is convenient for high-temperature dehydration together with the cooperation of calcium carbonate, polypropylene glycol and the like, and the difficult problem that the base material is thick and cannot be dehydrated is avoided.
PreferablyThe calcium carbonate comprises nano calcium carbonate and heavy calcium carbonate with the weight ratio of (1-3) 1, and the specific surface area of the nano calcium carbonate is 27+/-2 m 2 The/g stearic acid modified calcium and the heavy calcium carbonate is 1250-mesh calcium powder.
Preferably, the stabilizer is selected from the group consisting of a mixture of bis trimethoxy silyl ethane and a low basicity activated molecular sieve in a weight ratio of 1 (1-5). The chemical water removal and the physical adsorption water removal are matched together, so that a good storage effect is achieved. The low-alkalinity activated molecular sieve is preferably a Luoyang-building Long Weina JLH-PU activated molecular sieve. The low-alkalinity activated molecular sieve not only can assist the bis-trimethoxy silicon-based ethane to thoroughly remove water, but also can improve the storage stability of the product; moreover, compared with the common molecular sieve, the low-alkalinity characteristic has fewer side reactions; meanwhile, small molecules decomposed by aging can be adsorbed to slow down aging, so that the service life is prolonged.
Preferably, the silane coupling agent is selected from a mixture of JH-AP1231 and JH-OP17 in a weight ratio of 1:1, so that fewer small molecules are released in the curing process of the MS glue, thereby improving the moisture and heat resistance stability of the product.
Preferably, the anti-aging aid is selected from U-pack UV-7775. Liquid auxiliaries are more beneficial to adding and operating.
The invention also provides a preparation method of the weather-resistant MS door and window glue, which comprises the following steps: adding dimethoxy methylsilyl polyether polymer, diphenyl ketone modified oligomeric silsesquioxane, calcium carbonate, polypropylene glycol and anti-aging auxiliary agent into a dynamic mixer, stirring, vacuumizing, stirring, heating to 110 ℃ and dehydrating; and (3) after the temperature in the dynamic mixer kettle is reduced to below 50 ℃, adding trimethoxy STP polymer, stabilizer, silane coupling agent and catalyst step by step under the protection of nitrogen, uniformly mixing under the condition of vacuumizing, stopping the machine after the reaction is completed, filling nitrogen, releasing vacuum to normal pressure, and filling.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, specific types and proportions of MS polymers, calcium carbonate, polypropylene glycol, auxiliary agents, stabilizers, silane coupling agents and catalysts in the benzophenone modified oligomeric silsesquioxane and MS sealant are introduced for the first time, and the water ultraviolet resistance and the wet heat aging resistance of the product are synergistically improved.
Compared with the conventional silicone colloid system, the MS door and window colloid provided by the invention has the advantages that the alkane plasticizer of the silicone system is not contained, and components such as polypropylene glycol and a matched molecular sieve are used instead, so that the thermal weight loss of the product is lower, and the problem of volume shrinkage is reduced.
Detailed Description
The invention provides a weather-proof MS door and window adhesive and a preparation method thereof, and the weather-proof MS door and window adhesive is prepared by screening MS polymers, benzophenone modified oligomeric silsesquioxane, calcium carbonate, plasticizers, assistants, storage stabilizers, silane coupling agents and catalysts in specific types and proportions, and achieves the technical effects of lower thermal weight loss, volume shrinkage performance and effective improvement of water-resistant ultraviolet and humid heat aging performance.
The present invention will be described in further detail with reference to specific examples so as to more clearly understand the present invention by those skilled in the art. The following examples are given for illustration of the invention only and are not intended to limit the scope of the invention. All other embodiments obtained by those skilled in the art without creative efforts are within the protection scope of the present invention based on the specific embodiments of the present invention. In the examples of the present invention, all raw material components are commercially available products well known to those skilled in the art unless specified otherwise; in the embodiments of the present invention, unless specifically indicated, all technical means used are conventional means well known to those skilled in the art.
Partial raw material sources:
dimethoxymethylsilyl polyether type MS polymer, available from Brillouin chemical S810 resin, has an average viscosity of 18-23 Pa.s at 25deg.C.
trimethoxySTP type MS polymer is obtained from Ruiyanglitai 3368T resin and 30000T resin, and has average viscosity of 30-40 Pa.s at 25 ℃.
Polypropylene glycol, available from Shanghai eastern large chemical Co., ltd.
Stabilizing agent: low alkaline activated molecular sieves were purchased from Luoyang under Long Weina JLH-PU type.
Calcium carbonate: nano calcium carbonate (stearic acid modified calcium with specific surface area of 27 + -2 m 2/g) was purchased from Guangxi Huana New material Co. Heavy calcium carbonate (1250 mesh) was purchased from colone powder limited.
The silane coupling agent is selected from Jiang Han chemical JH-AP1231 and JH-OP17; an anti-aging aid selected from Li Anlong U-pack UV-7775.
Benzophenone-modified oligomeric silsesquioxanes, reference J.wuhanUniv.Vol.61No.1Feb.2015,067-072, comprises the following specific method steps: into a three-necked flask equipped with a thermometer and a reflux condenser, 16 parts of octachloropropyl cage type silsesquioxane was added to dissolve in dry DMF, followed by 25 parts of 4-hydroxybenzophenone, 3 parts of sodium iodide and 17 parts of anhydrous potassium carbonate. And (3) maintaining the temperature of 100 ℃ under the protection of argon for 8 hours, stopping the reaction, cooling and centrifuging. And taking supernatant, distilling under reduced pressure to remove DMF (dimethyl formamide) to obtain yellow viscous substance, dissolving the yellow viscous substance in dichloromethane, washing with water for 3 times to remove all residual potassium salt and sodium salt, separating an organic layer, and pumping the solvent to obtain the benzophenone-modified oligomeric silsesquioxane. The inner skeleton consists of an inorganic silica core, and the outer part is surrounded by 8 benzophenone groups.
Example 1
The embodiment provides a weather-resistant MS door and window adhesive, which is prepared from the following raw materials in parts by weight: 100 parts of MS polymer (50 parts of S810 resin, 50 parts of 3368T resin), 30 parts of benzophenone-modified oligomeric silsesquioxane, 280 parts of calcium carbonate (180 parts of nano calcium carbonate, 100 parts of heavy calcium carbonate), 90 parts of polypropylene glycol, 4 parts of UV-7775 auxiliary agent, 15 parts of storage stabilizer (10 parts of activated molecular sieve, 5 parts of bis trimethoxy silicon-based ethane), 7 parts of silane coupling agent (3.5 parts of JH-AP1231,3.5 parts of JH-OP 17) and 0.6 part of dibutyltin dilaurate.
The preparation method of the weather-resistant MS door and window glue of the embodiment comprises the following steps:
weighing the raw materials according to the proportion: adding the alkyl polyether type MS polymer S810 resin, the benzophenone modified oligomeric silsesquioxane, the calcium carbonate, the polypropylene glycol and the auxiliary agent into a dynamic mixer, stirring for 0.5h, vacuumizing and stirring, heating to 110 ℃ and dehydrating for 2h; after the temperature in the dynamic mixer kettle is reduced to below 50 ℃, STP type polymer resin, a storage stabilizer, a silane coupling agent and a catalyst are respectively added in steps every half an hour under the protection of nitrogen, the materials are uniformly mixed under the condition of vacuumizing, the machine is stopped after the reaction is completed, the nitrogen is filled, the vacuum is released to normal pressure, and the materials are quickly pressed into plastic packaging tubes to prepare the finished product.
Example 2
The embodiment provides a weather-resistant MS door and window adhesive, which is prepared from the following raw materials in parts by weight: 100 parts of MS polymer (65 parts of S810 resin, 35 parts of 3368T resin), 35 parts of benzophenone-modified oligomeric silsesquioxane, 350 parts of calcium carbonate (200 parts of nano calcium carbonate, 150 parts of heavy calcium carbonate), 90 parts of polypropylene glycol, 4 parts of UV-7775 auxiliary agent, 15 parts of storage stabilizer (10 parts of activated molecular sieve, 5 parts of bis trimethoxy silicon-based ethane), 7 parts of silane coupling agent (3.5 parts of JH-AP1231,3.5 parts of JH-OP 17) and 0.7 part of dibutyltin dilaurate.
The process steps of the preparation method of the weather-proof MS door and window glue of the embodiment are the same as those of the embodiment 1.
Example 3
The embodiment provides a weather-resistant MS door and window adhesive, which is prepared from the following raw materials in parts by weight: 100 parts of MS polymer (60 parts of S810 resin, 40 parts of 30000T resin), 39 parts of benzophenone-modified oligomeric silsesquioxane, 220 parts of calcium carbonate (110 parts of nano calcium carbonate, 110 parts of heavy calcium carbonate), 90 parts of polypropylene glycol, 4 parts of UV-7775 auxiliary agent, 19 parts of storage stabilizer (14 parts of activated molecular sieve, 5 parts of bis trimethoxy silicon-based ethane), 7 parts of silane coupling agent (3.5 parts of JH-AP1231,3.5 parts of JH-OP 17) and 0.8 part of dibutyltin dilaurate.
The process steps of the preparation method of the weather-proof MS door and window glue of the embodiment are the same as those of the embodiment 1.
Example 4
The embodiment provides a weather-resistant MS door and window adhesive, which is prepared from the following raw materials in parts by weight: 100 parts of MS polymer (65 parts of S810 resin, 35 parts of 30000T resin), 22 parts of benzophenone-modified oligomeric silsesquioxane, 380 parts of calcium carbonate (270 parts of nano calcium carbonate, 110 parts of heavy calcium carbonate), 80 parts of polypropylene glycol, 4 parts of UV-7775 auxiliary agent, 12 parts of storage stabilizer (14 parts of activated molecular sieve, 2 parts of bis trimethoxy silicon ethane), 5 parts of silane coupling agent (2.5 parts of JH-AP1231,2.5 parts of JH-OP 17) and 0.7 part of dibutyltin dilaurate.
The process steps of the preparation method of the weather-proof MS door and window glue of the embodiment are the same as those of the embodiment 1.
Comparative example 1
This comparative example provides an MS sealant having substantially the same composition as that of a weatherable MS door and window sealant of example 1, except that: an MQ silicone resin with a molar mass of 2000g/mol was used instead of benzophenone-modified oligomeric silsesquioxanes. The process steps of the preparation method of the MS sealant are the same as in example 1.
Comparative example 2
This comparative example provides an MS sealant having substantially the same composition as that of a weatherable MS door and window sealant of example 1, except that: the same amount of aminopropyl trimethoxysilane is used for replacing JH-AP1231, and the same amount of glycidol ether oxypropyl trimethoxysilane is used for replacing JH-OP17. The process steps of the preparation method of the MS sealant are the same as in example 1.
Comparative example 3
This comparative example provides an MS sealant having substantially the same composition as that of a weatherable MS door and window sealant of example 1, except that: the weight ratio of the S810 resin to the 3368T resin is 4:1.
Comparative example 4
This comparative example provides an MS sealant having substantially the same composition as that of a weatherable MS door and window sealant of example 4, except that: the weight ratio of S810 resin to 30000T resin was 1:4.
Performance testing
The MS sealant prepared in the test example is respectively subjected to performance test, and the test items and the test method comprise the following steps:
(1) Test items are tested according to the GB/T14683-20 HM method, the base material is anodized aluminum and glass with the thickness of 50mm or 50mm, the bonding area of 50mm or 12mm is prepared, and the test is carried out after 21 days of normal temperature maintenance.
(2) Room temperature tensile strength, tensile strength after water uv treatment, tensile strength after double 85 test: according to the GB16776 test method, water ultraviolet aging is carried out for 300 hours, double 85 aging is carried out for 500 hours, and after expiration, the steel is taken out and placed for 2 hours to normal temperature, and then the tensile strength is tested.
The statistics of the test results are shown in the following table:
MS sealant performance test result statistical table
As can be seen from table 1 above, compared with comparative example 1, the MS door and window adhesives prepared in examples 1 to 4 have both a tensile strength after water ultraviolet and a tensile strength after double 85 of above 0.7MPa, a strength retention after aging of above 75%, and a certain advantage in elastic recovery; the MS sealant products prepared in examples 1 to 4 showed less than 1.5% thermal weight loss, showing better environmental protection and volume retention, compared to comparative example 2. Therefore, the glue products of the embodiments 1 to 4 completely meet the standard requirements of the building industry GB/T14683, have the advantages of low thermal weight loss and excellent operation time, and can effectively improve the water ultraviolet resistance and the wet heat aging resistance.
In addition, it was found through a large number of studies that:
the use of benzophenone-modified oligomeric silsesquioxanes allows for a high degree of fusion with alkyl terminated MS polymers. When the MS door and window glue is irradiated by sunlight to undergo an aging reaction, the inorganic-organic hybrid compound can well play a role in nano-size, block or decompose consumed radiant energy, and protect an MS polymer system from aging, so that the oxidation resistance and the damp-heat resistance stability of the door and window glue are improved.
Further, the benzophenone modified oligomeric silsesquioxane is compounded with calcium carbonate, polypropylene glycol, an auxiliary agent, a stabilizer, a silane coupling agent and a catalyst which are matched in a specific type in cooperation with the alkyl-terminated MS polymer, so that the comprehensive properties such as proper operation time, low thermal weight loss, no shrinkage in volume, weather resistance (water ultraviolet resistance and humid heat aging resistance) and the like can be ensured to be more excellent.
It should be noted that the above examples are only for further illustrating and describing the technical solution of the present invention, and are not intended to limit the technical solution of the present invention, and the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The weather-resistant MS door and window glue is characterized by being prepared from the following raw materials in parts by weight:
100 parts of MS polymer, 20-40 parts of benzophenone modified oligomeric silsesquioxane, 200-400 parts of calcium carbonate, 80-120 parts of polypropylene glycol, 2-5 parts of anti-aging auxiliary agent, 10-20 parts of stabilizer, 5-9 parts of silane coupling agent and 0.3-1 part of catalyst;
wherein the MS polymer is selected from the following components in percentage by weight (1-3): 1 and trimethoxystp type polymer.
2. The weatherable MS window and door adhesive of claim 1, wherein the MS polymer is selected from the group consisting of (1 to 2.5) by weight: 1 and trimethoxystp type polymer.
3. The weather-resistant MS door and window adhesive according to claim 1 or 2, wherein the dimethoxymethylsilane-based polyether polymer is selected from S810 resin having an average viscosity of 18-23 Pa-S at 25 ℃;
the trimethoxySTP polymer 3368T resin and 30000T resin have average viscosity of 30-40 Pa.s at 25 ℃.
4. The weather-proof MS door and window glue according to claim 1 or 2, wherein the calcium carbonate comprises nano calcium carbonate and heavy calcium carbonate with the weight ratio of (1-3) 1, and the specific surface area of the nano calcium carbonate is 27+/-2 m 2 Stearic acid modified calcium/g, heavy calcium carbonate 1250 mesh calcium powder.
5. The weatherable MS window and door glue according to claim 1 or 2, wherein the stabilizer is selected from the group consisting of a mixture of bis trimethoxy silyl ethane and a low alkaline activated molecular sieve.
6. The weatherable MS window and door glue according to claim 5, wherein the stabilizer is selected from the group consisting of a mixture of (1-5) bis trimethoxy silyl ethane and a low alkalinity activated molecular sieve in a weight ratio of 1.
7. The weatherable MS window and door glue according to claim 1 or 2, wherein the silane coupling agent is selected from the group consisting of a mixture of JH-AP1231 and JH-OP17.
8. The weatherable MS window and door glue according to claim 7, wherein the silane coupling agent is selected from the group consisting of a mixture of JH-AP1231 and JH-OP17 in a weight ratio of 1:1.
9. The weather resistant MS door and window glue of claim 1 or 2, wherein the anti-aging aid is selected from the group consisting of U-pack UV-7775.
10. A method for preparing a weather-resistant MS door window adhesive according to any one of claims 1 to 9, comprising the steps of:
adding dimethoxy methylsilyl polyether polymer, diphenyl ketone modified oligomeric silsesquioxane, calcium carbonate, polypropylene glycol and anti-aging auxiliary agent into a dynamic mixer, stirring, vacuumizing, stirring, heating to 110 ℃ and dehydrating; and (3) after the temperature in the dynamic mixer kettle is reduced to below 50 ℃, adding trimethoxy STP polymer, stabilizer, silane coupling agent and catalyst step by step under the protection of nitrogen, uniformly mixing under the condition of vacuumizing, stopping the machine after the reaction is completed, filling nitrogen, releasing vacuum to normal pressure, and filling.
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