CN114539970A - Light-weight low-air-tightness two-component silicone sealant and preparation method thereof - Google Patents

Light-weight low-air-tightness two-component silicone sealant and preparation method thereof Download PDF

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CN114539970A
CN114539970A CN202210391258.3A CN202210391258A CN114539970A CN 114539970 A CN114539970 A CN 114539970A CN 202210391258 A CN202210391258 A CN 202210391258A CN 114539970 A CN114539970 A CN 114539970A
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weight
parts
component
light
silicone sealant
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Inventor
蔡耀武
陆瑜翀
李瑶
王珂
陶新良
曾荣平
史乾坤
孙小康
王亚豪
赵永振
徐坤
蔡建武
蔡新奇
张英才
刘东升
李衡彦
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Zhengzhou Hollowlite Materials Co ltd
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Zhengzhou Hollowlite Materials Co ltd
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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
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • 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
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B80/00Architectural or constructional elements improving the thermal performance of buildings
    • Y02B80/22Glazing, e.g. vaccum glazing

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a light-weight low-airtightness two-component silicone sealant which consists of a component A and a component B; the component A is prepared from the following raw materials: 50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane; 10-60 parts by weight of vinyl polydimethylsiloxane; 10-60 parts by weight of polyether polyol; 10-60 parts by weight of silicone oil; 10-30 parts by weight of a silane-terminated polyurethane polymer; 20-80 parts by weight of hollow glass beads; 10-150 parts by weight of a filler; the component B is prepared from the following raw materials: 50-150 parts by weight of silicone oil; 20-80 parts by weight of hollow glass beads; 0.5-25 parts by weight of carbon black; 10-150 parts by weight of a filler; 10-50 parts by weight of a crosslinking agent; 1-10 weight of coupling agentWeighing parts; 0.1-10 parts by weight of a catalyst; the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm. The light and low-airtightness two-component silicone sealant adopts specific components with specific contents, realizes better overall interaction, and has the advantages of low product density, good uniformity, high adhesion, bonding strength and hardness and good airtightness.

Description

Light-weight low-air-tightness two-component silicone sealant and preparation method thereof
Technical Field
The invention relates to the technical field of sealants, in particular to a light-weight low-airtightness two-component silicone sealant and a preparation method thereof.
Background
The hollow glass is energy-saving glass which is commonly applied to buildings such as commercial office buildings, superstores, high-rise houses and the like at present, has excellent heat insulation and sound insulation performance, and is attractive and practical. The hollow glass is formed by bonding two (or more) pieces of glass and a spacing strip, the sealing type mainly adopts a rubber strip method and a glue joint method, and the prior art adopts a double-channel sealing structure in the sealing structure of the glue joint method: two pieces of glass are separated by a spacing bar, the spacing bar and the glass are sealed close to the front by butyl rubber, a molecular sieve is filled in the spacing bar, and a gap formed between the edge of the glass and the outer side of the spacing bar is sealed by two sealant.
One sealant acts to prevent moisture or inert gas from entering and exiting the cavity, and butyl rubber is generally used because of its very low moisture permeability and inert gas permeability. But the butyl rubber has low bonding strength and small elasticity, and the whole structure must be fixed by two sealant layers to bond the glass plate and the spacing bar together, so that when the hollow glass bears load, one sealant layer can keep good sealing effect, and meanwhile, the whole structure is not influenced.
The second hollow glass sealant mainly comprises three types of polysulfide, polyurethane and silicone, wherein the polysulfide and the silicone are mainly used in the domestic market at present, and the polyurethane type is late in appearance and less in application in China.
The silicone sealant is a sealant taking polysiloxane as a main raw material. The high molecular chain of the silicone sealant mainly consists of Si-O-Si, and a reticular Si-O-Si framework structure is formed by crosslinking in the curing process. The Si-O bond energy (444KJ/mol) is very high, not only much larger than that of other polymers, but also larger than that of ultraviolet rays (399 KJ/mol). The molecular structure of the silicone sealant enables the silicone sealant to have the advantages of excellent high and low temperature resistance, weather resistance, ultraviolet aging resistance and the like, and the water absorption rate is low; the disadvantage of using for insulating glass is the high gas permeability.
In the prior art: patent grant publication no: CN 106190013B, patent name: a silicone resin type bi-component elastic silicone sealant for hollow glass and a preparation method thereof, wherein the preparation method comprises the following steps: 12 and 17 months in 2019. According to the invention, the flexible alkoxy silicon resin and the MQ silicon resin are added for synergistic action, so that the prepared silicone sealant has excellent elasticity, impact resistance, durable high-strength adhesive property, high peel strength, high mechanical strength, high and low temperature resistance, weather resistance, small compression set and other properties. But can not change the defect of high gas permeability of the silicone sealant.
Patent application No.: 21610982507.0, patent name: a two-component odor-removing hollow glass silicone sealant is disclosed in the application date: 2016, 11, 9 months. The product of the invention has good odor removing effect and strong bonding strength, and the bonding strength can reach 0.86MPa after detection that the content of micromolecular alcohols such as methanol, ethanol and the like is about 1 percent. The disadvantage of high gas permeability of silicone sealants cannot be changed.
Patent grant publication no: CN111057516B, patent name: a high-temperature curable silicone structural sealant and application thereof, wherein the sealant is issued on the notice day: 12 and 3 days 2021. The modified resin is added into the component B, so that the activity of the sealant can be improved. However, the addition thereof to component B results in poor storage stability of the sealant.
Disclosure of Invention
In view of the above, the invention aims to provide a light-weight low-air-tightness two-component silicone sealant and a preparation method thereof.
The invention provides a light-weight low-airtightness two-component silicone sealant which consists of a component A and a component B;
the component A is prepared from the following raw materials:
50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane;
10-60 parts by weight of vinyl polydimethylsiloxane;
10-60 parts by weight of polyether polyol;
10-60 parts by weight of silicone oil;
10-30 parts by weight of a silane-terminated polyurethane polymer;
20-80 parts by weight of hollow glass beads;
10-150 parts by weight of a filler;
the component B is prepared from the following raw materials:
50-150 parts by weight of silicone oil;
20-80 parts by weight of hollow glass beads;
0.5-25 parts by weight of carbon black;
10-150 parts by weight of a filler;
10-50 parts by weight of a crosslinking agent;
1-10 parts by weight of a coupling agent;
0.1-10 parts by weight of a catalyst;
the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm.
Preferably, the viscosity of the hydroxyl-terminated polydimethylsiloxane is 3000-100000 cp.
Preferably, the vinyl polydimethylsiloxane is terminal vinyl polydimethylsiloxane, and the viscosity is 200-1000 cp.
Preferably, the polyether polyol is selected from polyether diols and/or polyether triols; the molecular weight of the polyether glycol is 1000-5000 g/mol; the molecular weight of the polyether triol is 500-6000 g/mol.
Preferably, the viscosity of the silicone oil is 100-500 cp.
Preferably, the silane-terminated polyurethane polymer is selected from one or more of SPUR 1050MM, SPUR1015LM, SPUR Y-15987.
Preferably, the filler is selected from one or more of calcium carbonate, kaolin, talcum powder, fumed silica and mica powder.
Preferably, the specific surface area of the carbon black is 100-130 m2/g。
Preferably, the crosslinking agent is selected from one or more of polyalkoxysilane, polybutanone oxime silane, polyacetoxy silane, polyamine silane, polyamide silane and polyiso-acryloxy silane;
the coupling agent is a silane coupling agent with at least one group of amino, sulfydryl, vinyl, epoxy, cyano and methyl-propyl-vinyl-oxy;
the catalyst is selected from an organic tin catalyst and/or an organic bismuth catalyst.
The invention also provides a preparation method of the light-weight low-airtightness two-component silicone sealant, which comprises the following steps:
a) drying the hollow glass beads, the filler and the carbon black in a drying oven at 100-110 ℃ for 3-5 hours;
b) respectively carrying out vacuum-pumping dehydration on vinyl polydimethylsiloxane and polyether polyol for 2-3 h at the temperature of 110-120 ℃; slowly adding vinyl polydimethylsiloxane into polyether polyol, and carrying out vacuum pumping reaction for 2-3 h at the temperature of 80-100 ℃ to obtain polyether polyol grafted vinyl polydimethylsiloxane;
c) adding hydroxyl-terminated polydimethylsiloxane, polyether polyol grafted vinyl polydimethylsiloxane, silicone oil and silane-terminated polyurethane polymer into a double-planetary mixer, and stirring and mixing at the rotating speed of 20-40 HZ for 5-10 min; adding the dried filler, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component A;
d) adding silicone oil and the dried filler into a double-planet stirrer, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; adding a cross-linking agent, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding a coupling agent and a catalyst, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component B; the preparation of the light and low-air-tightness double-component silicone sealant is completed.
The invention provides a light-weight low-airtightness two-component silicone sealant which consists of a component A and a component B; the component A is prepared from the following raw materials: 50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane; 10-60 parts by weight of vinyl polydimethylsiloxane; 10-60 parts by weight of polyether polyol; 10-60 parts by weight of silicone oil; 10-30 parts by weight of a silane-terminated polyurethane polymer; 20-80 parts by weight of hollow glass beads; 10-150 parts by weight of a filler; the component B is prepared from the following raw materials: 50-150 parts by weight of silicone oil; 20-80 parts by weight of hollow glass beads; 0.5 to 25 parts by weight of carbon black; 10-150 parts by weight of a filler; 10-50 parts by weight of a crosslinking agent; 1-10 parts by weight of a coupling agent; 0.1-10 parts by weight of a catalyst; the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm. Compared with the prior art, the light-weight low-airtightness two-component silicone sealant provided by the invention adopts specific components with specific contents, realizes better overall interaction, has small product density, good uniformity, high adhesiveness, bonding strength and hardness and good airtightness, and can solve the problems of high density, difficult uniform mixing, poor airtightness compared with polysulfide sealant and polyurethane sealant and the like when the existing two-component silicone sealant is used for hollow glass two-component sealant.
In addition, the preparation method provided by the invention has the advantages of simple process, mild condition, easiness in control and wide application prospect.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
The invention provides a light-weight low-airtightness two-component silicone sealant which consists of a component A and a component B;
the component A is prepared from the following raw materials:
50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane;
10-60 parts by weight of vinyl polydimethylsiloxane;
10-60 parts by weight of polyether polyol;
10-60 parts by weight of silicone oil;
10-30 parts by weight of a silane-terminated polyurethane polymer;
20-80 parts by weight of hollow glass beads;
10-150 parts by weight of a filler;
the component B is prepared from the following raw materials:
50-150 parts by weight of silicone oil;
20-80 parts by weight of hollow glass beads;
0.5-25 parts by weight of carbon black;
10-150 parts by weight of a filler;
10-50 parts by weight of a crosslinking agent;
1-10 parts by weight of a coupling agent;
0.1-10 parts by weight of a catalyst;
the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm.
In the invention, the component A is prepared from the following raw materials:
50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane;
10-60 parts by weight of vinyl polydimethylsiloxane;
10-60 parts by weight of polyether polyol;
10-60 parts by weight of silicone oil;
10-30 parts by weight of a silane-terminated polyurethane polymer;
20-80 parts by weight of hollow glass beads;
10-150 parts by weight of a filler;
the compound is preferably prepared from the following raw materials:
70-80 parts by weight of hydroxyl-terminated polydimethylsiloxane;
30 parts by weight of vinyl polydimethylsiloxane;
10 parts of polyether polyol;
20 parts of silicone oil;
20-30 parts by weight of a silane-terminated polyurethane polymer;
30-40 parts by weight of hollow glass beads;
80-100 parts by weight of a filler.
In the invention, the viscosity of the hydroxyl-terminated polydimethylsiloxane is preferably 3000-100000 cp, and more preferably 80000 cp. The source of the hydroxyl-terminated polydimethylsiloxane is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the invention, the vinyl polydimethylsiloxane is preferably terminal vinyl polydimethylsiloxane, and the viscosity is preferably 200-1000 cp, and more preferably 500 cp. The source of the terminal vinyl polydimethylsiloxane is not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
In the present invention, the polyether polyol is preferably selected from polyether diols and/or polyether triols, more preferably polyether diols; the molecular weight of the polyether glycol is preferably 1000-5000 g/mol, and more preferably 1000 g/mol; the molecular weight of the polyether triol is preferably 500-6000 g/mol. The source of the polyether polyol in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used.
In the invention, the vinyl polydimethylsiloxane and the polyether polyol can form polyether polyol grafted vinyl polydimethylsiloxane, and the polyether polyol grafted vinyl polydimethylsiloxane is added, so that the surface hydrophilicity of the two-component silicone sealant can be improved, and the adhesion of the two-component silicone sealant can be improved.
In the present invention, the viscosity of the silicone oil is preferably 100 to 500cp, and more preferably 500 cp. The source of the silicone oil is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the silane-terminated polyurethane polymer is preferably selected from one or more of SPUR 1050MM, SPUR1015LM, SPUR Y-15987, and more preferably SPUR 1050 MM. In the invention, the silane-terminated polyurethane polymer is a modified resin prepared by the organosilicon oligomer and the polyurethane resin, has the advantages of high strength, high elongation at break and low water vapor transmission rate, and can improve the hardness and tensile strength of the sealant and reduce the water vapor transmission rate by introducing the silane-terminated polyurethane polymer into the existing hydroxyl-terminated polydimethylsiloxane curing system. According to the invention, the silane-terminated polyurethane polymer is added, so that the bonding strength and hardness of the two-component silicone sealant can be effectively improved, and the air tightness is reduced. The source of the silane-terminated polyurethane polymer is not particularly limited in the present invention and commercially available products well known to those skilled in the art may be used.
According to the invention, the silane end-capped polyurethane polymer is added into the component A, and the silane end-capped polyurethane polymer has good compatibility with the hydroxyl-terminated polydimethylsiloxane, so that the bonding strength and hardness of the two-component silicone sealant can be effectively improved, and the air tightness is reduced.
In the invention, the density of the hollow glass beads is preferably 0.12-0.7 g/cm3More preferably 0.4 to 0.48g/cm3The particle size is preferably 5 to 100 μm, more preferably 30 to 40 μm (D90). According to the invention, the hollow glass beads are added, so that the fluidity of the sealant can be increased, the uniform mixing is promoted, and the density is reduced. The source of the hollow glass beads is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the filler is preferably selected from one or more of calcium carbonate, kaolin, talc, fumed silica, mica powder, and more preferably calcium carbonate; in a preferred embodiment of the invention, the filler is stearic acid-treated nano calcium carbonate. The source of the filler in the present invention is not particularly limited, and commercially available products known to those skilled in the art may be used.
In the invention, the component B is prepared from the following raw materials:
50-150 parts by weight of silicone oil;
20-80 parts by weight of hollow glass beads;
0.5-25 parts by weight of carbon black;
10-150 parts by weight of a filler;
10-50 parts by weight of a crosslinking agent;
1-10 parts by weight of a coupling agent;
0.1-10 parts by weight of a catalyst;
the compound is preferably prepared from the following raw materials:
80 parts of silicone oil;
40-50 parts by weight of hollow glass beads;
8 parts by weight of carbon black;
80-100 parts by weight of a filler;
20 parts of a crosslinking agent;
5 parts of a coupling agent;
1 part by weight of catalyst.
In the present invention, the silicone oil, the hollow glass beads and the filler are the same as those in the above technical scheme, and are not described herein again.
In the invention, the carbon black is preferably MPC, and the specific surface area is preferably 100-130 m2(ii) g, more preferably 110m2(ii) in terms of/g. The carbon black of the present invention is not particularly limited in its source, and commercially available products known to those skilled in the art may be used.
In the present invention, the crosslinking agent is preferably selected from one or more of polyalkoxysilane, polybutanone oxime silane, polyacetoxysilane, polyaminosilane, polyamidosilane, polyisoacryloxysilane, and more preferably methyltributanone oxime silane; the coupling agent is preferably a silane coupling agent with at least one group of amino, mercapto, vinyl, epoxy, cyano and methyl-propionyloxy, more preferably KH 560; the catalyst is preferably selected from organotin-based catalysts and/or organobismuth-based catalysts, and more preferably dibutyltin dilaurate. The sources of the crosslinking agent, the coupling agent and the catalyst are not particularly limited in the present invention, and commercially available products well known to those skilled in the art may be used.
The light and low-airtightness two-component silicone sealant provided by the invention adopts specific components with specific contents, realizes better overall interaction, and particularly introduces hollow glass beads with specific conditions and parameter limitation, wherein the hollow glass beads are hollow spheres, the true density of the hollow glass beads is far lower than that of fillers such as calcium carbonate, the density of the hollow glass beads can be effectively reduced after the sealant is added, the dead weight of the hollow glass is reduced, meanwhile, the hollow glass beads are smooth spheres, compared with the fillers with other shapes, the flowability of the sealant component A and the component B can be increased, and the component A and the component B can be better and easily mixed uniformly in the mixing process; on the basis, the product has small density, good uniformity, high adhesiveness, bonding strength and hardness and good air tightness, and can solve the problems of large density, difficult uniform mixing, poor air tightness compared with polysulfide sealant and polyurethane sealant and the like when the existing two-component silicone sealant is used for hollow glass secondary sealant.
The invention also provides a preparation method of the light-weight low-airtightness two-component silicone sealant, which comprises the following steps:
a) drying the hollow glass beads, the filler and the carbon black in a drying oven at 100-110 ℃ for 3-5 hours;
b) respectively carrying out vacuum-pumping dehydration on vinyl polydimethylsiloxane and polyether polyol for 2-3 h at the temperature of 110-120 ℃; slowly adding vinyl polydimethylsiloxane into polyether polyol, and carrying out vacuum pumping reaction for 2-3 h at the temperature of 80-100 ℃ to obtain polyether polyol grafted vinyl polydimethylsiloxane;
c) adding hydroxyl-terminated polydimethylsiloxane, polyether polyol grafted vinyl polydimethylsiloxane, silicone oil and silane-terminated polyurethane polymer into a double-planetary mixer, and stirring and mixing at the rotating speed of 20-40 HZ for 5-10 min; adding the dried filler, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component A;
d) adding silicone oil and the dried filler into a double-planet stirrer, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; adding a cross-linking agent, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding a coupling agent and a catalyst, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component B; the preparation of the light and low-air-tightness double-component silicone sealant is completed.
The preparation method provided by the invention has the advantages of simple process, mild condition, easiness in control and wide application prospect.
The invention provides a light-weight low-airtightness two-component silicone sealant which consists of a component A and a component B; the component A is prepared from the following raw materials: 50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane; 10-60 parts by weight of vinyl polydimethylsiloxane; 10-60 parts by weight of polyether polyol; 10-60 parts by weight of silicone oil; 10-30 parts by weight of a silane-terminated polyurethane polymer; 20-80 parts by weight of hollow glass beads; 10-150 parts by weight of a filler; the component B is prepared from the following raw materials: 50-150 parts by weight of silicone oil; 20-80 parts by weight of hollow glass beads; 0.5-25 parts by weight of carbon black; 10-150 parts by weight of a filler; 10-50 parts by weight of a crosslinking agent; 1-10 parts by weight of a coupling agent; 0.1-10 parts by weight of a catalyst; the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm. Compared with the prior art, the light-weight low-airtightness two-component silicone sealant provided by the invention adopts specific components with specific contents, realizes better overall interaction, has small product density, good uniformity, high adhesiveness, high bonding strength and hardness and good airtightness, and can solve the problem that the existing two-component silicone sealant is used for preparing the sealantWhen the second sealant is used for the hollow glass, the problems of high density, difficult uniform mixing, poor air tightness compared with polysulfide sealant and polyurethane sealant and the like exist.
In addition, the preparation method provided by the invention has the advantages of simple process, mild condition, easiness in control and wide application prospect.
To further illustrate the present invention, the following examples are provided for illustration. The raw materials used in the following examples of the present invention are all commercially available products.
Example 1
The formula composition of the light-weight low-airtightness two-component silicone sealant provided by the embodiment is as follows:
Figure BDA0003597019820000101
Figure BDA0003597019820000111
the preparation method comprises the following steps:
(1) and drying the hollow glass beads, the filler and the carbon black in a drying oven at 100-110 ℃ for 4 hours.
(2) The vinyl polydimethylsiloxane and the polyether glycol are respectively vacuumized and dehydrated for 2.5 hours at the temperature of 110-120 ℃. Slowly adding the vinyl polydimethylsiloxane into the polyether glycol, and carrying out vacuum pumping reaction for 2.5h at the temperature of 90 ℃ to obtain the polyether glycol grafted vinyl polydimethylsiloxane.
(3) Adding hydroxyl-terminated polydimethylsiloxane, polyether glycol grafted vinyl polydimethylsiloxane, silicone oil and silane-terminated polyurethane polymer into a double-planetary stirrer, and stirring and mixing for 8min at the rotating speed of 30 HZ; adding the dried filler, stirring for 6min at 30HZ, switching to high-speed 40HZ stirring, starting vacuum, and continuously stirring for 1.5h under the vacuum condition (the vacuum degree is 0.09 +/-0.05 MPa); then adding the dried hollow glass beads, stirring for 6min at 25HZ, starting vacuum, and continuously stirring for 20min at the rotating speed of 25HZ under the vacuum condition (the vacuum degree is 0.09 +/-0.05 MPa); and finally, filling nitrogen gas to discharge the glue to a packaging bottle to obtain the component A product.
(4) Adding silicone oil and the dried filler into a double-planet stirrer, stirring for 6min at 30HZ, switching to high-speed 40HZ stirring, starting vacuum, and continuously stirring for 1.5h under the vacuum condition (the vacuum degree is 0.09 +/-0.05 MPa); adding the cross-linking agent, and continuously stirring for 20min at the rotating speed of 40HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding a coupling agent and a catalyst, and continuously stirring for 20min at the rotating speed of 40HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 5min at 25HZ, starting vacuum, and continuously stirring for 20min at the rotating speed of 25HZ under the vacuum condition (the vacuum degree is 0.09 +/-0.05 MPa); finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component B product; the preparation of the light and low-air-tightness double-component silicone sealant is completed.
Example 2
The formula composition of the light-weight low-airtightness two-component silicone sealant provided by the embodiment is as follows:
Figure BDA0003597019820000112
Figure BDA0003597019820000121
the specific preparation method is the same as that of the example 1, and the light-weight and low-air-tightness two-component silicone sealant is obtained.
Example 3
The formula composition of the light-weight low-airtightness two-component silicone sealant provided by the embodiment is as follows:
Figure BDA0003597019820000122
Figure BDA0003597019820000131
the specific preparation method is the same as that of the example 1, and the light-weight and low-air-tightness two-component silicone sealant is obtained.
Comparative example 1
The formulation composition is shown in the following table:
Figure BDA0003597019820000132
the specific preparation method is the same as that of the example 1, and the two-component silicone sealant is obtained.
Comparative example 2
The formulation composition is shown in the following table:
Figure BDA0003597019820000141
the specific preparation method is the same as that of the example 1, and the two-component silicone sealant is obtained.
The light and low-air-tightness two-component silicone sealant provided in the embodiments 1-3 and the two-component silicone sealant provided in the comparative examples 1-2 are tested for various performances, wherein the extrusion property testing method comprises the following steps: 10: 1 mixing rubber tube, 345ml in volume, 24 sections of mixing nozzle, 0.34MPa in air pressure setting and 1min in test time, and testing five groups of data to obtain an arithmetic mean value.
The results are shown in the following table:
Figure BDA0003597019820000142
the previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A light and low-airtightness two-component silicone sealant consists of a component A and a component B;
the component A is prepared from the following raw materials:
50-200 parts by weight of hydroxyl-terminated polydimethylsiloxane;
10-60 parts by weight of vinyl polydimethylsiloxane;
10-60 parts by weight of polyether polyol;
10-60 parts by weight of silicone oil;
10-30 parts by weight of a silane-terminated polyurethane polymer;
20-80 parts by weight of hollow glass beads;
10-150 parts by weight of a filler;
the component B is prepared from the following raw materials:
50-150 parts by weight of silicone oil;
20-80 parts by weight of hollow glass beads;
0.5-25 parts by weight of carbon black;
10-150 parts by weight of a filler;
10-50 parts by weight of a crosslinking agent;
1-10 parts by weight of a coupling agent;
0.1-10 parts by weight of a catalyst;
the density of the hollow glass beads is 0.12-0.7 g/cm3The particle size is 5 to 100 μm.
2. The light-weight, low-air-tightness two-component silicone sealant as claimed in claim 1, wherein the hydroxyl-terminated polydimethylsiloxane has a viscosity of 3000-100000 cp.
3. The light-weight low-airtightness two-component silicone sealant as claimed in claim 1, wherein the vinyl polydimethylsiloxane is a terminal vinyl polydimethylsiloxane, and the viscosity is 200-1000 cp.
4. The light, low air-tightness two-component silicone sealant according to claim 1, wherein the polyether polyol is selected from polyether diols and/or polyether triols; the molecular weight of the polyether glycol is 1000-5000 g/mol; the molecular weight of the polyether triol is 500-6000 g/mol.
5. The light-weight low-airtightness two-component silicone sealant as claimed in claim 1, wherein the viscosity of the silicone oil is 100-500 cp.
6. The light, low air-tightness two-component silicone sealant according to claim 1, wherein said silane-terminated polyurethane polymer is selected from one or more of SPUR 1050MM, SPUR1015LM, SPUR Y-15987.
7. The light weight, low air permeability two component silicone sealant of claim 1 wherein the filler is selected from one or more of calcium carbonate, kaolin, talc, fumed silica, mica powder.
8. The light-weight low-airtightness two-component silicone sealant as claimed in claim 1, wherein the specific surface area of the carbon black is 100-130 m2/g。
9. The light, low air barrier two-component silicone sealant of claim 1 wherein said cross-linking agent is selected from one or more of the group consisting of polyalkoxysilanes, polybutanonemethoxysilanes, polyacetoxysilanes, polyamines silanes, polyamides silanes, polyisoacryloxysilanes;
the coupling agent is a silane coupling agent with at least one group of amino, sulfydryl, vinyl, epoxy, cyano and methyl-propyl-vinyl-oxy;
the catalyst is selected from an organic tin catalyst and/or an organic bismuth catalyst.
10. A method for preparing a light-weight, low-air-tightness two-component silicone sealant as claimed in any one of claims 1 to 9, comprising the steps of:
a) drying the hollow glass beads, the filler and the carbon black in a drying oven at 100-110 ℃ for 3-5 hours;
b) respectively carrying out vacuum-pumping dehydration on vinyl polydimethylsiloxane and polyether polyol for 2-3 h at the temperature of 110-120 ℃; slowly adding vinyl polydimethylsiloxane into polyether polyol, and carrying out vacuum pumping reaction for 2-3 h at the temperature of 80-100 ℃ to obtain polyether polyol grafted vinyl polydimethylsiloxane;
c) adding hydroxyl-terminated polydimethylsiloxane, polyether polyol grafted vinyl polydimethylsiloxane, silicone oil and silane-terminated polyurethane polymer into a double-planetary mixer, and stirring and mixing at the rotating speed of 20-40 HZ for 5-10 min; adding the dried filler, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component A;
d) adding silicone oil and the dried filler into a double-planet stirrer, stirring for 3-10 min at 20-40 HZ, switching to high-speed stirring at 30-50 HZ, starting vacuum, and continuously stirring for 1-2 h under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; adding a cross-linking agent, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding a coupling agent and a catalyst, and continuously stirring for 10-30 min at the rotating speed of 30-50 HZ under the vacuum degree of 0.09 +/-0.05 MPa; then adding the dried hollow glass beads, stirring for 3-10 min at 20-30 HZ, starting vacuum, and continuously stirring for 10-30 min at the rotating speed of 20-30 HZ under the vacuum condition that the vacuum degree is 0.09 +/-0.05 MPa; finally, filling nitrogen gas to discharge glue to a packaging bottle to obtain a component B; the preparation of the light and low-air-tightness double-component silicone sealant is completed.
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Cited By (2)

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CN115029003A (en) * 2022-07-14 2022-09-09 歌尔股份有限公司 Liquid silica gel, silica gel part and electronic equipment
CN115466595A (en) * 2022-11-07 2022-12-13 河南瑞朗达新材料有限公司 Bi-component modified silicone rubber adhesive for bonding automobile cabin door and preparation method and bonding process thereof

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Publication number Priority date Publication date Assignee Title
CN102352214A (en) * 2011-08-05 2012-02-15 曾庆铭 Double-component silicone structural sealant

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN102352214A (en) * 2011-08-05 2012-02-15 曾庆铭 Double-component silicone structural sealant

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115029003A (en) * 2022-07-14 2022-09-09 歌尔股份有限公司 Liquid silica gel, silica gel part and electronic equipment
CN115466595A (en) * 2022-11-07 2022-12-13 河南瑞朗达新材料有限公司 Bi-component modified silicone rubber adhesive for bonding automobile cabin door and preparation method and bonding process thereof
CN115466595B (en) * 2022-11-07 2024-04-02 河南瑞朗达新材料有限公司 Bi-component modified silicone rubber adhesive for bonding automobile cabin door, preparation method and bonding process thereof

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