CN111073576B - High-functional silane modified polyether sealant - Google Patents
High-functional silane modified polyether sealant Download PDFInfo
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- CN111073576B CN111073576B CN201911251562.2A CN201911251562A CN111073576B CN 111073576 B CN111073576 B CN 111073576B CN 201911251562 A CN201911251562 A CN 201911251562A CN 111073576 B CN111073576 B CN 111073576B
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- modified polyether
- functional silane
- silane modified
- catalyst
- polyether sealant
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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
- C09J171/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/336—Polymers modified by chemical after-treatment with organic compounds containing silicon
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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
- 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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a high-functional silane modified polyether sealant which has better fluidity, aging resistance and stain resistance under the condition of higher filler content, and the raw materials of the sealant comprise the following components in percentage by weight: 10-15% of high-functional silane modified polyether resin, 0.05-0.5% of perfluoroalkyl alcohol, 60-70% of filler, 1-5% of thixotropic agent, 1-3% of dehydrating agent, 0.02-0.08% of first catalyst, 8-15% of plasticizer, 0.10-0.40% of ultraviolet absorbent, 0-3% of coloring agent, 0.5-1.0% of coupling agent, 0.04-0.1% of antioxidant and 0.4-1.0% of flame retardant.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a high-functional silane modified polyether sealant.
Background
The silane modified polyether resin is also called MS resin, is an alkoxy silane terminated polyether resin, can be hydrolyzed, crosslinked and cured under the action of a catalyst and water to generate a macromolecular elastomer, has low modulus, high elastic recovery rate, good adhesion and better water resistance and aging resistance, is prepared into a mixture with a plasticizer, a filler, a coloring agent, a catalyst, an anti-aging agent and a flame retardant, can be used for sealing gaps of inner and outer walls of an assembled building or sealing of vehicles, mechanical equipment, doors and windows, glass curtain walls and the like, and is called MS sealant in the industry. When the MS resin is used outdoors, particularly applied to outer walls, the MS resin is required to have excellent durability, stain resistance and mechanical property, and the common MS resin is difficult to meet the long-term use requirement. The problems can be solved to a certain extent by improving the filler content and reducing the resin content, but the indexes such as better fluidity, elastic recovery rate and the like are difficult to ensure under the condition of high filler content in the conventional MS sealant, and the filler content is usually controlled within the range of 40-45%.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a high-functional silane modified polyether sealant which has better fluidity, aging resistance and stain resistance under the condition of higher filler content.
The high-functional silane modified polyether sealant comprises the following components in percentage by weight:
10-15% of high-functional silane modified polyether resin, 0.05-0.5% of perfluoroalkyl alcohol, 60-70% of filler, 1-5% of thixotropic agent, 1-3% of dehydrating agent, 0.02-0.08% of first catalyst, 8-15% of plasticizer, 0.10-0.40% of ultraviolet absorbent, 0-3% of coloring agent, 0.5-1.0% of coupling agent, 0.04-0.1% of antioxidant and 0.4-1.0% of flame retardant.
The high-functional silane modified polyether sealant provided by the embodiment of the invention has at least the following beneficial effects:
the perfluoroalkyl alcohol has certain lubricity, is beneficial to improving the content of the filler, and ensures the fluidity, the wear resistance, the aging resistance and the stain resistance of the system; the high-functional silane modified polyether resin can improve the crosslinking degree, and redundant hydroxyl after hydrolysis can react with the hydroxyl of perfluoroalkyl alcohol, so that the long-term stability is improved, the influence on the toughness due to overhigh crosslinking degree is avoided, and the use requirement of the building outer wall can be well met.
The highly functional silane-modified polyether resin preferably has a functionality of 4 or more, and according to some embodiments of the present invention, is prepared as follows:
and (2) dehydrating polypropylene glycol under the heating condition in vacuum, charging nitrogen, adding isocyanatopropyl triethoxysilane and a second catalyst to ensure that-NCO is excessive relative to-OH, reacting until NCO% is basically stable, and distilling under reduced pressure to prepare the high-functional silane modified polyether resin.
According to some embodiments of the invention, the second catalyst is dibutyltin bisacetylacetonate and/or bismuth neodecanoate.
According to some embodiments of the invention, the second catalyst is prepared by compounding dibutyltin bisacetylacetonate and bismuth neodecanoate according to the molar ratio of 1-3: 1, so that the catalytic efficiency is higher.
According to some embodiments of the invention, the reaction temperature is 120 to 130 ℃.
According to some embodiments of the invention, the polypropylene glycol has a molecular weight of 12000-15000.
According to some embodiments of the invention, the determination of% NCO is by the di-n-butylamine method.
According to some embodiments of the invention, the perfluoroalkyl alcohol is perfluorohexylethanol.
According to some embodiments of the invention, the first catalyst is dibutyltin bisacetylacetonate.
According to some embodiments of the invention, the plasticizer is diisooctyl phthalate and/or diisononyl phthalate.
According to some embodiments of the invention, the filler comprises quartz powder, organically modified silica micropowder, and sericite powder. The content of the quartz powder is preferably 20-40% and the particle size is preferably 60-150 meshes, wherein the total weight of the filler is 100%, and the quartz powder is used as a volume filler and a colorant; the organic modified silicon micro powder is used as a main inorganic filler, the content is preferably 35-55%, the particle size is preferably 300-800 meshes, and the oil absorption is less than 30g/100 g; the content of the sericite powder is preferably 10-25%, the particle size is preferably 300-600 meshes, and the specific surface is 30-80 m2And/g, besides the increment function, the sericite powder can also improve the ultraviolet resistance, water resistance and aging resistance of the sealant.
According to some embodiments of the invention, the coupling agent is KH-792.
According to some embodiments of the invention, the flame retardant is microencapsulated red phosphorus.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the following detailed description is further provided in conjunction with specific embodiments. The embodiments described herein are only some of the embodiments of the present application and should not be construed as limiting the scope of the present application.
In the following examples and comparative examples, the perfluoroalkyl alcohol was perfluorohexylethanol; 120 meshes of quartz sand, 400 meshes of organic modified silicon micropowder and 600 meshes of sericite powder; the first catalyst is dibutyltin bisacetylacetonate; the thixotropic agent is fumed silica; dehydrating agent vinyltrimethoxysilane; ultraviolet light absorber Cotosll UV713 and antioxidant CotosllKy-1635, all available from Nanjing Ketone chemical Co., Ltd; a coupling agent KH-792; the flame retardant microcapsule red phosphorus is purchased from Qingdao Changrong chemical Co Ltd; the plasticizer is diisooctyl phthalate and diisononyl phthalate; the colorant is rutile titanium dioxide with the particle size of 100 nm.
The preparation method of the high-functional silane modified polyether resin comprises the following steps:
vacuum dehydrating polypropylene glycol (with molecular weight of 15000) at 120 ℃ until the water content is lower than 0.05%, charging nitrogen, adding isocyanatopropyl triethoxysilane and a second catalyst, reacting at constant temperature until the NCO% is basically stable, and distilling under reduced pressure to obtain the high-functional silane modified polyether resin; wherein, the molar ratio of the polypropylene glycol to the isocyanatopropyl triethoxysilane is 1:2.2, the second catalyst is dibutyltin bisacetylacetonate and bismuth neodecanoate with the molar ratio of 2:1, the dosage is 0.03 percent of the molar number of the polypropylene glycol, and the NCO percent determination method is a di-n-butylamine method. At present, most of MS resin in the market is monopolized by foreign companies such as Japan and the like, the price is higher, and the embodiment adopts a simple method to synthesize the high-functionality MS resin, so that the use requirement of the sealant can be met, and the resin cost is reduced.
The sealant formulations of examples 1-2 are shown in Table 1 and were prepared as follows:
(1) weighing the components in parts by weight, adding the high-functional silane modified polyether resin, perfluoroalkyl alcohol, plasticizer and antioxidant into stainless steel mixing equipment with a planetary mixer, wherein the equipment has the functions of stirring, temperature regulation, vacuumizing, charging and discharging, sealing, stirring, adding thixotropic agent, and continuing stirring;
(2) sealing the equipment, vacuumizing to-0.09 MPa, and heating to 100%
Stirring for 60 minutes at 10 ℃; adding a dehydrating agent and a coupling agent, and stirring for 15 minutes;
(3) adding the filler into the quartz powder, the active silicon micro powder and the sericite powder in sequence, continuing stirring for 15 minutes after the filler is added, adding the colorant, and stirring for 10 minutes;
(4) transferring the mixture to a three-roll grinder to grind for 3 times, adding the ground mixture into a planetary stirrer to continue stirring for 15 minutes, and cooling to 40 DEG
10℃；
(5) Adding an ultraviolet absorbent, a flame retardant and a first catalyst, and stirring for 30 minutes;
(6) and (5) removing vacuum, pressing, packaging and sealing to obtain the sealant.
TABLE 1 (parts by weight)
Comparative example
Compared with the examples, the difference is that the perfluoroalkyl alcohol is not contained.
The sealant performance of the examples and comparative examples were tested and the results are shown in table 2, wherein:
the tensile shear strength and the elongation at break adopt GB/T528-2009 standard;
the Shore A hardness adopts GB/T531-2008 standard, and the viscosity is measured at 25 ℃ by adopting Brookfield LVDV digital display rotational viscometer;
the artificial aging test refers to GB/T16422-2014 standard, and the average irradiance is 0.5W/m2Plate temperature 65
The test time is 1000 hours at 2 ℃, after the artificial aging test, the sample is air-dried for 24 hours at room temperature, and the elastic recovery rate and the tensile shear strength are tested;
the rest of the test items are tested according to the relevant regulations of GB/T14683.
TABLE 2
Claims (9)
1. The high-functional silane modified polyether sealant is characterized by comprising the following components in percentage by weight:
10-15% of high-functional silane modified polyether resin, 0.05-0.5% of perfluoroalkyl alcohol, 60-70% of filler, 1-5% of thixotropic agent, 1-3% of dehydrating agent, 0.02-0.08% of first catalyst, 8-15% of plasticizer, 0.10-0.40% of ultraviolet absorbent, 0-3% of coloring agent, 0.5-1.0% of coupling agent, 0.04-0.1% of antioxidant and 0.4-1.0% of flame retardant; the perfluoroalkyl alcohol is perfluorohexylethanol.
2. The high-functional silane-modified polyether sealant according to claim 1, wherein the high-functional silane-modified polyether resin is prepared by the following method:
and (2) dehydrating polypropylene glycol under the heating condition in vacuum, charging nitrogen, adding isocyanatopropyl triethoxysilane and a second catalyst to ensure that-NCO is excessive relative to-OH, reacting until NCO% is basically stable, and distilling under reduced pressure to prepare the high-functional silane modified polyether resin.
3. The highly functional silane modified polyether sealant of claim 2, wherein the second catalyst is dibutyltin bisacetylacetonate and/or bismuth neodecanoate.
4. The high-functional silane modified polyether sealant as claimed in claim 3, wherein the second catalyst is prepared by compounding dibutyltin bisacetylacetonate and bismuth neodecanoate according to a molar ratio of 1-3: 1.
5. The high-functional silane modified polyether sealant according to claim 2, wherein the reaction temperature is 120-130 ℃.
6. The high-functional silane-modified polyether sealant according to claim 2, wherein the polypropylene glycol has a molecular weight of 12000-15000.
7. The highly functional silane modified polyether sealant of claim 1, wherein the first catalyst is dibutyltin bisacetylacetonate.
8. The high functionality silane modified polyether sealant according to claim 1, wherein the plasticizer is diisooctyl phthalate and/or diisononyl phthalate.
9. The high-functional silane-modified polyether sealant according to claim 1, wherein the filler comprises quartz powder, organically modified silica micropowder and sericite powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911251562.2A CN111073576B (en) | 2019-12-09 | 2019-12-09 | High-functional silane modified polyether sealant |
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| CN201911251562.2A CN111073576B (en) | 2019-12-09 | 2019-12-09 | High-functional silane modified polyether sealant |
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| CN111073576B true CN111073576B (en) | 2022-04-19 |
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