CN114437658A - Silane modified polyether sealant and preparation method and application thereof - Google Patents

Silane modified polyether sealant and preparation method and application thereof Download PDF

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CN114437658A
CN114437658A CN202111600357.XA CN202111600357A CN114437658A CN 114437658 A CN114437658 A CN 114437658A CN 202111600357 A CN202111600357 A CN 202111600357A CN 114437658 A CN114437658 A CN 114437658A
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modified polyether
sealant
component
silane
parts
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崔巍
周傲
王玺
刘铁军
李锡慧
魏慧男
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China Construction Technology Group Beijing Low Carbon Smart City Technology Co ltd
Shenzhen Graduate School Harbin Institute of Technology
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China Construction Technology Group Beijing Low Carbon Smart City Technology Co ltd
Shenzhen Graduate School Harbin Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J171/00Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention provides a silane modified polyether sealant as well as a preparation method and application thereof, and relates to the technical field of sealants. The silane modified polyether sealant provided by the invention comprises a component A and a component B which are independently packaged, wherein the component A comprises silane modified polyether resin, a first plasticizer, calcium carbonate, titanium dioxide and/or graphene and a light stabilizer; the component B comprises a second plasticizer, carbon black, a silane coupling agent and an organic metal catalyst. The sealant provided by the invention has the advantages of low modulus, small internal stress, high bonding strength with concrete and high curing speed. The titanium dioxide can effectively improve the ultraviolet resistance of the sealant, can reflect most ultraviolet rays and delay the aging time of the sealant; the graphene can fill up the pores generated during the curing of the sealant, reduce the water absorption of the sealant and improve the water resistance of the sealant. The sealant provided by the invention has more excellent mechanical property, ultraviolet resistance and water resistance, and has a very good application prospect in fabricated buildings.

Description

Silane modified polyether sealant and preparation method and application thereof
Technical Field
The invention relates to the technical field of sealants, in particular to a silane modified polyether sealant and a preparation method and application thereof.
Background
The fabricated building has the advantages of energy saving, material saving, shortened construction period, environmental protection and the like, and occupies a larger area in the building. The assembly type building adopts a factory prefabrication field assembly mode, 2-3 cm wide splicing seams can be reserved in the assembly process, and the splicing seams need sealant with excellent performance to be filled. In addition, sealants are widely used in exterior walls of fabricated buildings. Currently, sealants for fabricated buildings are traditional silicone sealants, polyurethane sealants and silicone modified polyether (MS) sealants. The traditional silicone sealant has high modulus and poor pollution resistance; the polyurethane sealant has poor weather resistance and is easy to crack; the MS sealant has the advantages of both silicone sealant and polyurethane sealant, has the advantages of good adhesion, weather resistance, flexibility, coating property and the like, and is most widely applied.
Chinese patent CN110903809A discloses a weather-resistant sealant for an assembled building outer wall, which consists of the following substances: the silane modified polyether type light stabilizer comprises silane modified polyether, a filler, a plasticizer, a thixotropic agent, a catalyst, a water removing agent, a light stabilizer, an antioxidant and an ultraviolet absorber, wherein the filler is one or more of nano calcium carbonate, coarse whiting, titanium dioxide, quartz sand, graphene and carbon black, the plasticizer is one or more of phthalate, phosphate and fatty acid ester, the thixotropic agent is fumed silica, the catalyst is one or more of organic tin, chelated tin and ammonia, and the water removing agent is one or two of vinyl trimethoxy silane and vinyl triethoxy silane. However, the sealant is a single-component sealant, is cured by moisture in the air, has a slow curing speed, and is mainly applied to curtain wall glass. The high-tensile modulus concrete member has high tensile modulus and internal stress, and is easy to cause sealant cracking when applied to concrete members and deformed joints.
Disclosure of Invention
In view of the above, the invention aims to provide a silane modified polyether sealant and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a variety of silane modified polyether sealants, which comprise a component A and a component B which are independently packaged;
the component A comprises the following preparation raw materials in parts by mass: 11-13 parts of silane modified polyether resin, 12-14 parts of a first plasticizer, 28-33 parts of calcium carbonate, 0.25-2.4 parts of an auxiliary agent and 0.1-0.3 part of a light stabilizer; the auxiliary agent comprises titanium dioxide and/or graphene;
the component B comprises the following raw materials in parts by mass: 44-46 parts of a second plasticizer, 9-11 parts of carbon black, 3-5 parts of a silane coupling agent and 2-4 parts of an organic metal catalyst.
Preferably, the first and second plasticizers independently comprise diisononyl phthalate and/or diisodecyl phthalate.
Preferably, the calcium carbonate comprises nano calcium carbonate and ground calcium carbonate; the mass ratio of the nano calcium carbonate to the heavy calcium carbonate is 19-21: 9-11; the particle size of the nano calcium carbonate is 90-120 nm; the granularity of the heavy calcium carbonate is 1000-1500 meshes.
Preferably, the light stabilizer is a hindered amine light stabilizer.
Preferably, the silane coupling agent comprises gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
Preferably, the organometallic catalyst comprises a chelated tin catalyst.
The invention provides a preparation method of the silane modified polyether sealant in the technical scheme, which comprises the following steps:
(1) mixing silane modified polyether resin, a first plasticizer, calcium carbonate, an auxiliary agent and a light stabilizer to obtain a component A;
(2) mixing a second plasticizer, carbon black, a silane coupling agent and an organic metal catalyst to obtain a component B;
(3) independently subpackaging the component A and the component B to obtain the silane modified polyether sealant;
the step (1) and the step (2) have no time sequence.
The invention also provides application of the silane modified polyether sealant in the technical scheme or the silane modified polyether sealant prepared by the preparation method in the technical scheme in an assembly type building.
Preferably, the mass ratio of the component A to the component B in the application process is 12-14: 1.
preferably, the silane modified polyether sealant is cured before use, the curing temperature is 20-25 ℃, and the relative humidity is 45-55%.
The invention provides a silane modified polyether sealant, which comprises a component A and a component B which are independently subpackaged; the component A comprises the following preparation raw materials in parts by mass: 11-13 parts of silane modified polyether resin, 12-14 parts of a first plasticizer, 28-33 parts of calcium carbonate, 0.25-2.4 parts of an auxiliary agent and 0.1-0.3 part of a light stabilizer; the auxiliary agent comprises titanium dioxide and/or graphene; the component B comprises the following raw materials in parts by mass: 44-46 parts of a second plasticizer, 9-11 parts of carbon black, 3-5 parts of a silane coupling agent and 2-4 parts of an organic metal catalyst. The surface of a concrete member is relatively loose, the silane modified polyether sealant provided by the invention has low tensile modulus and is soft, when the same deformation occurs, the internal stress of the silane modified polyether sealant is much smaller than that of a sealant product with the same displacement grade and high modulus, the condition that the sealant is cracked due to large internal stress can be effectively avoided, and the bonding strength with the concrete is high. The silane modified polyether sealant provided by the invention is a two-component sealant, and in the application process, an organic metal catalyst is simultaneously used as a curing agent, so that the curing speed of the component A and the component B is high, and the component A and the component B do not need to be cured by depending on moisture in the air. The titanium dioxide can effectively improve the anti-ultraviolet energy of the silane modified polyether sealant, the titanium dioxide has smaller crystal lattice and tighter combination, the combination is a more compact space network structure, the stability is good, the refractive index is high, most ultraviolet rays can be reflected, and the aging time of the silane modified polyether sealant is delayed; the graphene can fill up the pores generated during the curing of the silane modified polyether sealant, reduce the number of the defects of the pores of the formed sealing coating, reduce the water absorption of the sealing coating, and further improve the water resistance of the silane modified polyether sealant by the hydrophobic property and the change of the surface structure of the silane modified polyether resin. The addition of the carbon black, the titanium dioxide, the calcium carbonate and the graphene in the silane modified polyether sealant provided by the invention improves the mechanical property, the ultraviolet resistance and the water resistance of the sealant, prolongs the service life while ensuring the safety of an assembly type building, can save a large amount of maintenance cost, and has a very good application prospect in the assembly type building.
The invention provides a preparation method of the silane modified polyether sealant in the technical scheme. The preparation method provided by the invention is simple to operate, and the prepared silane modified polyether sealant is stable in comprehensive performance and suitable for industrial production.
Drawings
FIG. 1 is a graph showing tensile strength test results of silane modified polyether sealants prepared in examples 1 to 3 and comparative example 1;
FIG. 2 is a graph showing the results of elongation at break tests of the silane-modified polyether sealants prepared in examples 1 to 3 and comparative example 1;
FIG. 3 is a graph showing the results of water contact angle measurements of the silane-modified polyether sealants prepared in examples 1-3 and comparative example 1;
FIG. 4 is a graph of the results of the hydrophobic angle test of the silane modified polyether sealants prepared in examples 4-8 and comparative example 2.
Detailed Description
The invention provides a silane modified polyether sealant, which comprises a component A and a component B which are independently subpackaged;
the component A comprises the following preparation raw materials in parts by weight: 11-13 parts of silane modified polyether resin, 12-14 parts of a first plasticizer, 28-33 parts of calcium carbonate, 0.25-2.4 parts of an auxiliary agent and 0.1-0.3 part of a light stabilizer; the auxiliary agent comprises titanium dioxide and/or graphene;
the component B comprises the following preparation raw materials in parts by weight: 44-46 parts of a second plasticizer, 9-11 parts of carbon black, 3-5 parts of a silane coupling agent and 2-4 parts of an organic metal catalyst.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
The silane modified polyether sealant provided by the invention comprises a component A, wherein the component A comprises the following preparation raw materials in parts by weight: 11-13 parts of silane modified polyether (MS) resin, preferably 11.5-12.5 parts, and more preferably 12 parts. The silane-modified polyether (MS) resin of the present invention is not particularly limited, and commercially available silicon products well known to those skilled in the art may be used, specifically, silyl terminated polyether; in a specific embodiment of the present invention, the silane-modified polyether resin is preferably S203H. In the invention, the silane modified polyether resin has excellent adhesion, weather resistance and environmental protection, and can exert excellent mechanical properties after a moisture curing reaction process.
The component A is prepared from 12-14 parts of a first plasticizer, preferably 12.5-13.5 parts of the first plasticizer, and more preferably 13 parts of the first plasticizer. In the present invention, the first plasticizer preferably includes diisononyl phthalate (DINP) and/or diisodecyl phthalate (DIDP). In the invention, the plasticizer has the functions of weakening intermolecular force, reducing the viscosity and tensile modulus of the silane modified polyether sealant and improving the workability.
The preparation raw material of the component A comprises 28-33 parts of calcium carbonate, preferably 29-32 parts of calcium carbonate, and more preferably 30-31 parts of calcium carbonate in parts by weight of the silane-modified polyether resin. In the present invention, the calcium carbonate preferably includes nano calcium carbonate and ground calcium carbonate; the mass ratio of the nano calcium carbonate to the heavy calcium carbonate is preferably 19-21: 9 to 11, more preferably 19.5 to 20.5: 9.5-10.5, and more preferably 20: 10; the particle size of the nano calcium carbonate is preferably 90-120 nm, and more preferably 100-110 nm; the particle size of the heavy calcium carbonate is preferably 1000-1500 meshes, more preferably 1100-1400 meshes, and further preferably 1200-1300 meshes. In the invention, the calcium carbonate is used as a reinforcing agent, and the ground calcium carbonate is mainly used for adjusting the rheological property of the silane modified polyether sealant.
The preparation raw material of the component A comprises 0.25-2.4 parts of an auxiliary agent, preferably 0.5-2 parts, and more preferably 1-1.5 parts by mass of the silane modified polyether resin. In the invention, the auxiliary agent comprises titanium dioxide and/or graphene, and when the auxiliary agent is titanium dioxide, the mass part of the titanium dioxide is preferably 0.6-1.8 parts, preferably 0.8-1.6 parts, more preferably 1-1.4 parts, and further preferably 1.2-1.3 parts. In the invention, the granularity of the titanium dioxide is preferably 0.3-0.5 μm, and more preferably 0.35-0.45 μm. In the invention, when the auxiliary agent is graphene, the mass part of the graphene is preferably 0.25 to 0.6 part, preferably 0.3 to 0.55 part, more preferably 0.35 to 0.5 part, and further preferably 0.4 to 0.45 part. In the invention, when the auxiliary agent is titanium dioxide and graphene, the mass ratio of the titanium dioxide to the graphene is preferably 0.6-1.8: 0.25 to 0.6, more preferably 0.8 to 1.6: 0.3 to 0.55, and more preferably 1 to 1.4: 0.4 to 0.5. The traditional ultraviolet absorbers (such as ultraviolet absorbers UV326, light stabilizers 770 and antioxidants 1010) mainly absorb ultraviolet rays to convert energy, so that the conventional ultraviolet absorbers can cause damage to the sealant after being used for a long time, and reduce the ultraviolet resistance of the sealant. The titanium dioxide is used as the uvioresistant additive, the uvioresistant energy of the silane modified polyether sealant can be effectively improved by the titanium dioxide, the titanium dioxide is small in lattice and compact in combination, the combination body is a compact space network structure, the stability is good, the refractive index is high, most ultraviolet rays can be reflected, and the aging time of the silane modified polyether sealant is prolonged. In the invention, the doping of the graphene can fill up the pores generated during the curing of the silane modified polyether sealant, reduce the number of the pore defects of the formed sealing coating, reduce the water absorption of the sealing coating, and further improve the water resistance of the silane modified polyether sealant by the self hydrophobicity and changing the surface structure of the silane modified polyether resin.
The component A is prepared from 0.1-0.3 part of light stabilizer, preferably 0.15-0.25 part of light stabilizer, and more preferably 0.2 part of silane modified polyether resin. In the present invention, the light stabilizer is preferably a hindered amine light stabilizer, more preferably Tinuvin770 DF. In the invention, the light stabilizer effectively absorbs ultraviolet light, so that the silane modified polyether sealant is not damaged by light under long-term exposure.
The silane modified polyether sealant provided by the invention comprises a component B, wherein the component B comprises the following preparation raw materials in parts by weight: 44-46 parts of a second plasticizer, 9-11 parts of carbon black, 3-5 parts of a silane coupling agent and 2-4 parts of an organic metal catalyst.
The preparation raw material of the component B comprises 44-46 parts of a second plasticizer, preferably 44.5-45.5 parts, and more preferably 45 parts by mass of the silane modified polyether resin. In the present invention, the second plasticizer preferably includes diisononyl phthalate (DINP) and/or diisodecyl phthalate (DIDP). In the invention, the second plasticizer has the functions of weakening intermolecular force, reducing the viscosity and modulus of the silane modified polyether sealant and improving the workability.
The preparation raw material of the component B comprises 9-11 parts of carbon black, preferably 9.5-10.5 parts, and more preferably 10 parts by mass of the silane modified polyether resin. In the present invention, the carbon black functions as coloring; meanwhile, the modified polyether sealant can be used as a light absorbent to prevent the silane modified polyether sealant from photooxidation caused by sunlight irradiation.
The component B is prepared from 3-5 parts of silane coupling agent, preferably 3.5-4.5 parts of silane coupling agent, and more preferably 4 parts of silane modified polyether resin. In the present invention, the silane coupling agent preferably includes gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane (KH-560). In the invention, the silane coupling agent is used for improving the adhesive property and the elongation at break of the silane modified polyether sealant to the substrate.
The preparation raw material of the component B comprises 2-4 parts of organic metal catalyst, preferably 2.5-3.5 parts, and more preferably 3 parts by mass of the silane modified polyether resin. In the present invention, the organometallic catalyst preferably comprises a chelated tin catalyst, more preferably chelated tin U-220H. In the invention, the organic metal catalyst has the function of accelerating the vulcanization of the silane modified polyether sealant liquid, and the construction engineering efficiency of the silane modified polyether sealant is improved.
The invention provides a preparation method of the silane modified polyether sealant in the technical scheme, which comprises the following steps:
(1) mixing silane modified polyether resin, a first plasticizer, calcium carbonate, titanium dioxide, graphene and a light stabilizer to obtain a component A;
(2) mixing a second plasticizer, carbon black, a silane coupling agent and an organic metal catalyst to obtain a component B;
(3) independently subpackaging the component A and the component B to obtain the silane modified polyether sealant;
the step (1) and the step (2) have no time sequence.
According to the invention, the component A is obtained by mixing silane modified polyether resin, a first plasticizer, calcium carbonate, titanium dioxide, graphene and a light stabilizer. In a specific embodiment of the present invention, the mixing is preferably performed by first mixing the silane-modified polyether resin, the first plasticizer, the calcium carbonate, and the light stabilizer, second mixing the obtained first mixture with the titanium dioxide, and third mixing the obtained second mixture with the graphene. In the present invention, the first mixing preferably includes normal pressure stirring, dispersing and mixing, vacuum pumping and vacuum stirring, dispersing and mixing which are sequentially performed; the temperature of the first mixing is preferably 60-80 ℃, more preferably 65-75 ℃, and further preferably 70 ℃; the first mixing is preferably carried out in a planetary mixer in a stirring and dispersing way, and the rotating speed of the planetary mixer is preferably 400-800 r/min, and more preferably 500-600 r/min; the time for stirring, dispersing and mixing under normal pressure is preferably 5-15 min, more preferably 8-12 min, and further preferably 10 min; the vacuum degree after vacuumizing is preferably-0.08 to-0.1 MPa, and more preferably-0.09 MPa; the time for the vacuum stirring, dispersing and mixing is preferably 1-1.5 h, more preferably 1.1-1.4 h, and even more preferably 1.2-1.3 h. In the present invention, the second mixing is preferably performed by ultrasonic dispersion, and the ultrasonic dispersion is preferably performed by using an ultrasonic disperser; the ultrasonic power of the second mixing is preferably 600-1000W, more preferably 700-900W, and further preferably 800W; the second mixing time is preferably 30-40 min, more preferably 32-38 min, and even more preferably 34-35 min. In the present invention, the graphene is preferably used in the form of a graphene dispersion liquid, the third mixing is preferably performed by dispersing the graphene in an organic solvent to obtain a graphene dispersion liquid, and stirring and mixing the obtained graphene dispersion liquid and the second mixture; the organic solvent preferably comprises acetone, and the concentration of the graphene dispersion liquid is preferably 1.5-2.5 g/L, and more preferably 2 g/L; the dispersing mode is preferably ultrasonic dispersing, the ultrasonic dispersing is preferably carried out by using an ultrasonic disperser, the ultrasonic power of the ultrasonic dispersing is preferably 800-1200W, more preferably 900-1000W, and further preferably 900W, the time of the ultrasonic dispersing is preferably 30-40 min, more preferably 32-38 min, and further preferably 34-35 min; the stirring and mixing speed and time are not particularly limited, and the raw materials can be uniformly mixed and the organic solvent is completely volatilized.
According to the invention, a second plasticizer, carbon black, a silane coupling agent and an organic metal catalyst are mixed to obtain a component B. In the present invention, the mixing is preferably performed by vacuum agitation mixing, and the vacuum agitation mixing is preferably performed in a planetary agitator; the temperature of the mixing is preferably room temperature; the mixing rotating speed is preferably 400-800 r/min, and more preferably 500-600 r/min; the mixing time is preferably 1 to 1.5 hours, more preferably 1.1 to 1.4 hours, and even more preferably 1.2 to 1.3 hours.
After the component A and the component B are obtained, the component A and the component B are independently packaged to obtain the silane modified polyether sealant. The independent dispensing method is not particularly limited, and the dispensing method known to those skilled in the art can be adopted.
The invention provides the application of the silane modified polyether sealant in the technical scheme or the silane modified polyether sealant obtained by the preparation method in the technical scheme in an assembly type building.
In the invention, the mass ratio of the component A to the component B in the application process is preferably 12-14: 1, more 12.5-13.5: 1, more preferably 13: 1.
In the invention, the silane modified polyether sealant is cured before use, and the curing temperature is preferably 20-25 ℃, more preferably 21-24 ℃, and further preferably 22-23 ℃; the relative humidity of the curing treatment is preferably 45-55%, more preferably 48-52%, and further preferably 50%; the curing time is preferably 24 hours; the maintenance is preferably carried out in a constant temperature and humidity box; the temperature control range of the constant temperature and humidity box is preferably 5-60 ℃, and more preferably 20-50 ℃; the humidity control range of the constant temperature and humidity box is preferably 40-90%, and more preferably 50-80%.
In the present invention, the method of application preferably comprises the steps of: and respectively curing the component A and the component B, mixing, and coating the obtained cured silane modified polyether sealant on the fabricated building for curing again. In the present invention, the conditions for re-curing are preferably the same as the curing conditions described above, and will not be described herein again.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Placing 1.2g of titanium dioxide in an ultrasonic disperser, ultrasonically dispersing for 15min at 23 ℃ and 800W to obtain a first mixture, placing the first mixture, 24g of MS resin, 26g of DINP, 40g of nano calcium carbonate with the granularity of 90-120 nm, 20g of heavy calcium carbonate (heavy calcium) and 0.4g of Tinuvin770DF in a planetary mixer, stirring and dispersing for 10min at normal pressure under the condition, vacuumizing, and then stirring and dispersing for 1h at 70 ℃ and 600r/min in vacuum to obtain a component A;
placing 6.1g DINP, 1.3g carbon black, 0.5g KH-560 and 0.05g chelated tin U-220H in a planetary mixer, vacuumizing, and mixing for 1H under vacuum at 25 deg.C and 600r/min to obtain component B.
And (3) independently subpackaging the component A and the component B to obtain the silane modified polyether sealant.
Examples 2 to 8
The silane modified polyether sealant is prepared according to the method of the embodiment 1, and the preparation raw materials of the embodiments 2 to 8 are shown in table 1, wherein the first plasticizer in the embodiments 1 to 9 is DINP, and the second plasticizer in the embodiments 1 to 9 is DINP; in comparative example 1, the first plasticizer was DIDP and the second plasticizer was DIDP; in comparative example 2, the first plasticizer was DIDP and the second plasticizer was DIDP.
Comparative examples 1 to 2
The silane modified polyether sealant is prepared according to the method of example 1, and the preparation raw materials of comparative examples 1-2 are shown in Table 1.
TABLE 1 preparation raw materials for examples 1 to 8 and comparative examples 1 to 2
Figure BDA0003432926040000091
Comparative example 3
The silane modified polyether sealant is prepared according to the method of Chinese patent CN 110903809A.
Preparing raw materials: 20g of STPE-E30 silane modified polyether, 20g of graphene, 15g of heavy calcium carbonate, 10g of carbon black, 15g of tricresyl phosphate, 5g of epoxy fatty acid methyl ester, 3g of fumed silica, 0.5g of chelated tin, 1g of dodecamine, 2g of vinyl trimethoxy silane, 2g of light stabilizer (schoff), 2g of antioxidant (schoff) and 2g of ultraviolet absorber (schoff).
The method comprises the following specific steps:
the method comprises the following steps: mixing, heating and dispersing STPE-E30 silane modified polyether, graphene, heavy calcium carbonate, carbon black, tricresyl phosphate, epoxy fatty acid methyl ester and fumed silica, vacuumizing and dehydrating for 2 hours at the heating temperature of 100 ℃; step two: cooling to 50 deg.C, adding vinyltrimethoxysilane, chelated tin, dodecamine, light stabilizer, antioxidant and ultraviolet absorbent, dispersing at high speed for 0.5h, stirring under vacuum for 0.5h, and sealing and packaging.
Test example 1
The component A and the component B in the silane modified polyether sealants prepared in the examples 1 to 8 and the comparative examples 1 to 4 are respectively placed in a constant temperature and humidity box (400mm multiplied by 300mm multiplied by 400mm, the volume is 50L), standing and curing are carried out for 24H under the conditions of 23 ℃ and 50% RH, then the component A and the component B are stirred and mixed uniformly according to the mass ratio of 14:1, then the mixture is placed in a mold, then the mold is placed in an HWS-50B constant temperature and humidity box, and standing and curing are carried out for 14 days under the conditions of 23 ℃ and 50% RH, so that H-shaped test pieces with the thickness of 50mm multiplied by 12mm are obtained.
Testing the tensile property of the silane modified polyether sealant of an H-shaped test piece according to GB/T13477-2017 building sealing material test method, wherein the test method comprises the following steps: the test pieces were pulled to failure by a universal tester at a speed of (5.5. + -. 0.7) mm/min under a (23. + -. 2 ℃ C.) environment, and the tensile modulus was the force value at the selected elongation divided by the initial test cross-sectional area of the test piece, and the test results are shown in Table 2 and FIG. 1. FIG. 1 is a graph showing the tensile strength test results of the silane modified polyether sealants prepared in examples 1-3 and comparative example 1.
The test piece was pulled to failure at a speed of (5.5. + -. 0.7) mm/min in an environment of (23. + -. 2 ℃ C.) by a universal testing machine, and the elongation at break E was E ═ W1-W0)/W0,W0Is the preliminary test width of the test piece, W1The results of the elongation at break test are shown in table 2 and fig. 2, which are the widths at which the test pieces fail. FIG. 2 is a graph showing the results of elongation at break tests of the silane-modified polyether sealants prepared in examples 1 to 3 and comparative example 1.
Continuously irradiating the H-shaped test piece with ultraviolet light for 300H under the condition of no water immersionThe surface temperature of the test piece is 40 ℃, the power of the lamp tube is 300W, the lamp tube is parallel to the bottom of the box, the distance from the H-shaped test piece is 250mm, and the ultraviolet radiation intensity is 2500 mu W/cm2The glass surface of the H-shaped test piece was directed toward the light source, and the test results are shown in table 2.
The test piece was placed on a wetting angle measuring instrument, and the hydrophobic angle was measured by dropping water on the surface of the solid sample, with the water contact angle being shown in table 2 and fig. 3 to 4. FIG. 3 is a graph showing the results of water contact angle tests on the silane-modified polyether sealants prepared in examples 1 to 3 and comparative example 1, and FIG. 4 is a graph showing the results of hydrophobic angle tests on the silane-modified polyether sealants prepared in examples 4 to 8 and comparative example 2. If the sealant is in cohesive failure, the bonding strength cannot be measured, and the tensile strength value is consistent with the cohesive strength.
TABLE 2 Performance test results of silane-modified polyether sealants prepared in examples 1 to 8 and comparative examples 1 to 4
Figure BDA0003432926040000111
As can be seen from table 2 and fig. 1 to 4, when example 1 and example 9 are compared, DINP increases the tensile strength of the sealant, but slightly decreases the elongation at break, compared to DIDP. By comparing examples 1-3 with comparative example 1, when the content of titanium dioxide is 2%, the tensile strength of the sealant is increased to some extent, and is increased by 32% compared with the sealant without titanium dioxide; when the content of the titanium dioxide is 1% and 3%, the tensile strength is reduced to some extent; the elongation at break of the sealant after the titanium dioxide is added is improved compared with that of the sealant without the titanium dioxide, and when the addition amount of the titanium dioxide is 1%, 2% and 3%, the elongation at break of the sealant is respectively improved by 50%, 27% and 23%; the sealant chain scission elongation rate is gradually reduced along with the increase of the titanium dioxide content; after 2% of titanium dioxide is added, the tensile modulus of the sealant is improved by 32%; when the addition amount of the titanium dioxide is 1%, 2% and 3%, the hydrophobic angle of the sealant is increased by 8.3%, 13.7% and 18.6%, respectively, and the hydrophobic performance of the sealant is excellent. By comparing examples 4-8 with comparative example 2, when the addition amount of the graphene is 1%, the water contact angle of the sealant is reduced by 29.4%, and the water resistance is remarkably improved; when the addition amounts of the graphene are 0.4%, 0.6%, 0.8% and 1%, the contact angles of the sealant are respectively improved by 6.9%, 19.6%, 22.5% and 29.4%, and the sealant has excellent hydrophobic property.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The silane modified polyether sealant is characterized by comprising a component A and a component B which are independently packaged;
the component A comprises the following preparation raw materials in parts by weight: 11-13 parts of silane modified polyether resin, 12-14 parts of a first plasticizer, 28-33 parts of calcium carbonate, 0.25-2.4 parts of an auxiliary agent and 0.1-0.3 part of a light stabilizer; the auxiliary agent comprises titanium dioxide and/or graphene;
the component B comprises the following preparation raw materials in parts by weight: 44-46 parts of a second plasticizer, 9-11 parts of carbon black, 3-5 parts of a silane coupling agent and 2-4 parts of an organic metal catalyst.
2. The silane-modified polyether sealant of claim 1, wherein the first plasticizer and the second plasticizer independently comprise diisononyl phthalate and/or diisodecyl phthalate.
3. The silane modified polyether sealant of claim 1, wherein the calcium carbonate comprises nano calcium carbonate and ground calcium carbonate; the mass ratio of the nano calcium carbonate to the heavy calcium carbonate is 19-21: 9-11; the particle size of the nano calcium carbonate is 90-120 nm; the granularity of the heavy calcium carbonate is 1000-1500 meshes.
4. The silane modified polyether sealant according to claim 1, wherein the light stabilizer is a hindered amine light stabilizer.
5. The silane modified polyether sealant of claim 1, wherein the silane coupling agent comprises gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
6. The silane-modified polyether sealant of claim 1 wherein the organometallic catalyst comprises a chelated tin catalyst.
7. The preparation method of the silane modified polyether sealant as claimed in any one of claims 1 to 6, which is characterized by comprising the following steps:
(1) mixing silane modified polyether resin, a first plasticizer, calcium carbonate, an auxiliary agent and a light stabilizer to obtain a component A;
(2) mixing a second plasticizer, carbon black, a silane coupling agent and an organic metal catalyst to obtain a component B;
(3) independently subpackaging the component A and the component B to obtain the silane modified polyether sealant;
the step (1) and the step (2) have no time sequence.
8. The use of the silane-modified polyether sealants as claimed in any of claims 1 to 6 or of the silane-modified polyether sealants obtainable by the process as claimed in claim 7 in fabricated buildings.
9. The application of the composition as claimed in claim 8, wherein the mass ratio of the component A to the component B in the application process is 12-14: 1.
10. the application of claim 7 or 8, wherein the silane modified polyether sealant is cured before use, and the curing temperature is 20-25 ℃ and the relative humidity is 45-55%.
CN202111600357.XA 2021-12-24 2021-12-24 Silane modified polyether sealant and preparation method and application thereof Pending CN114437658A (en)

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* Cited by examiner, † Cited by third party
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CN115093828A (en) * 2022-07-19 2022-09-23 江苏江永新材料科技有限公司 Antifogging MS (Mass Spectrometry) automobile lamp sealant

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CN110951435A (en) * 2019-12-13 2020-04-03 成都硅宝科技股份有限公司 High-strength silane modified polyether sealant with equal proportion and preparation method thereof
WO2021232819A1 (en) * 2020-05-21 2021-11-25 广州市白云化工实业有限公司 Single-component silane-modified polyether sealant for prefabricated buildings and preparation method therefor

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CN108893061A (en) * 2018-07-12 2018-11-27 广西德本仕密封材料有限公司 A kind of weather-proof dual-component silicane modified polyether seal glue and preparation method thereof
CN110951435A (en) * 2019-12-13 2020-04-03 成都硅宝科技股份有限公司 High-strength silane modified polyether sealant with equal proportion and preparation method thereof
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