WO2018040952A1 - Modified white graphene-compounded butyl sealant for hollow glass and sealing method therefor - Google Patents

Modified white graphene-compounded butyl sealant for hollow glass and sealing method therefor Download PDF

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WO2018040952A1
WO2018040952A1 PCT/CN2017/098057 CN2017098057W WO2018040952A1 WO 2018040952 A1 WO2018040952 A1 WO 2018040952A1 CN 2017098057 W CN2017098057 W CN 2017098057W WO 2018040952 A1 WO2018040952 A1 WO 2018040952A1
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parts
white graphene
modified white
sealant
weight
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PCT/CN2017/098057
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French (fr)
Chinese (zh)
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段曦东
李晓丰
毛志浩
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广东纳路纳米科技有限公司
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Publication of WO2018040952A1 publication Critical patent/WO2018040952A1/en

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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
    • 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
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
    • C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
    • 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
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
    • C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
    • C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
    • 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
    • C08K2201/008—Additives improving gas barrier properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/14—Gas barrier composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Definitions

  • the invention relates to the technical field of sealant, in particular to a modified white graphene composite butyl sealant for insulating glass and a sealing method thereof.
  • Insulating glass sealant is the main factor determining the quality performance of insulating glass. Insulating glass insulation, sound insulation and frost-proof performance are realized by a layer of sealed and dry air inside. Therefore, one of the most important indicators for the selection of insulating glass sealants is the gas permeability and water vapor transmission rate of the sealing material. Whether it is the traditional slotted aluminum hollow glass or the new composite adhesive strip hollow glass, the selection and use of the sealant is the most important link.
  • Insulating glass on the market today is achieved by double-pass sealing.
  • Its inner sealant usually uses a non-vulcanized thermoplastic butyl sealant material, which is characterized by extremely low gas permeability, thus maintaining the internal air drying when the gas inside and outside the insulating glass is exchanged, but its adhesion And the strength does not meet the required requirements, and the complete seal cannot be achieved, so it must be guaranteed by the second sealing material.
  • Polysulfide sealant or silicone sealant is commonly used in the market as the second sealing material for insulating glass. This material can be well matched with the inner sealant and the glass and metal frame that is in contact with it. It has good compatibility and has certain strength, elasticity and good aging properties.
  • the first butyl sealant is subjected to a great test, and the butyl sealant has a gas and water vapor permeability. Without further strengthening, over time, water vapor easily penetrates into the hollow layer of the hollow glass through the sealant layer, causing frost and fog on the surface of the glass, which affects the service life of the insulating glass.
  • the present invention adopts the following technical solutions:
  • the modified white graphene composite butyl sealant for insulating glass of the invention comprises: a base rubber and an auxiliary agent;
  • the base rubber comprises 20 to 60 parts by weight of butyl rubber and 30 to 70 parts of polyisobutylene;
  • the auxiliary agent comprises: 5 to 30 parts by weight of a tackifier, 5 to 20 parts of a softener, 0.1 to 10 parts of a silane coupling agent, 0.01 to 5 parts of a modified white graphene, and 10 to 50 parts by weight. Strong filler, 0.01 ⁇ 5 parts anti-aging agent;
  • the montene rubber has a Mooney viscosity of 20 to 80, and the mixing processing effect is optimal;
  • the polyisobutylene has a number average molecular weight of 10,000 to 80,000, and the medium molecular weight is suitable for the substrate as a sealing material, and the sealing and bonding effects are optimal.
  • the base rubber comprises: 30 to 50 parts by weight of butyl rubber and 40 to 60 parts of polyisobutylene;
  • the auxiliary agent comprises: 5 to 20 parts by weight of a tackifier, 5 to 10 parts of a softener, 0.5 to 5 parts of a silane coupling agent, 0.01 to 2 parts of a modified white graphene, and 10 to 40 parts by weight. Strong filler, 0.01 to 3 parts of anti-aging agent.
  • the butyl rubber has a Mooney viscosity of 50; and the polyisobutylene has a number average molecular weight of 20,000.
  • the tackifier is one of coumarone resin, epoxy resin, and rosin;
  • the softener is petrolatum
  • the silane coupling agent is one of KH-550, KH-560, and KH-570;
  • the reinforcing filler is one of talc, light calcium carbonate and carbon black;
  • the anti-aging agent is one of the anti-aging agent D, the anti-aging agent 124, and the anti-aging agent NBC.
  • a sealing method for modified white graphene composite butyl sealant for insulating glass comprising:
  • Step 1) White graphene modification: 1-10 layers of white graphene with a surface percentage of 0.1% by mass The active agent is immersed for 24 hours, and the modified white graphene powder is obtained by centrifugation and vacuum drying;
  • Step 2) kneading of the base rubber: weighing the butyl rubber and the polyisobutylene in parts by weight in a vacuum kneader, and kneading at 90 to 150 ° C for 30 to 150 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: weigh a certain amount of tackifier, softener, silane coupling agent, modified white graphene powder, reinforcing filler and The antioxidant is added to the base rubber after mixing, mixed and stirred in a vacuum kneader to maintain a vacuum of 0.09 MPa, and mixed and stirred at 90 to 150 ° C for 30 to 120 minutes to obtain a modified white graphene composite butyl for hollow glass.
  • Base sealant is added to the base rubber after mixing, mixed and stirred in a vacuum kneader to maintain a vacuum of 0.09 MPa, and mixed and stirred at 90 to 150 ° C for 30 to 120 minutes to obtain a modified white graphene composite butyl for hollow glass.
  • Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass by a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to be 100 to 150 ° C. Achieve the desired sealing effect.
  • the surfactant described in step 1) is a long chain Lewis base, a long chain Lewis acid, a sulfonate, a quaternary amine, a nonionic surfactant.
  • the long-chain Lewis base is oleylamine or the like; the long-chain Lewis acid is long-chain borane or the like; the sulfonate is sodium dodecylbenzenesulfonate or the like; and the quaternary amination It is cetylpyridinium bromide or the like; the nonionic surfactant is a polyethylene oxide alkyl alcohol amide or the like.
  • the kneading component has a kneading temperature of 100 to 140 ° C, and the kneading time is 60 to 120 min; and in step 4), the hot melt adhesive extruder has an extrusion temperature of 110 to 140 ° C.
  • 1 ⁇ 10 layers of modified white graphene are selected as the modified particles of butyl sealant.
  • the layers are compact and uniform, and the number of barrier sheets is large.
  • the water vapor circulates in the butyl sealant, and the path becomes long and small. Adding can well block the passage of water vapor, effectively increase the airtightness of butyl rubber; at the same time, adding a small amount of white graphene treated by surfactant can achieve good wettability with the matrix, which can enhance the effect and improve The bond strength of butyl rubber.
  • the invention further enhances the barrier property of the first butyl sealant for insulating glass to gas and water vapor, effectively avoids the frosting and fogging phenomenon of the insulating glass after a long time of use, and prolongs the service life of the insulating glass. It is very suitable for hot melt extruder operation, green, with permanent plasticity and high applicability.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of petrolatum, 1 part of silane coupling agent KH-550, 0.1 part of modified white graphite are weighed by weight The olefin powder, 40 parts of light calcium carbonate and 0.5 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the modified glass is obtained.
  • White graphene composite butyl sealant 10 parts of coumarone resin, 5 parts of petrolatum, 1 part of silane coupling agent KH-550, 0.1 part of modified white graphite are weighed by weight The olefin powder, 40 parts of light calcium carbonate and 0.5 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110
  • Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C to further Sealing effect.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-550, 0.5 parts of modified white graphite are weighed by weight The olefin powder, 30 parts of light calcium carbonate and 1 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the hollow glass is modified.
  • White graphene composite butyl sealant 10 parts of coumarone resin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-550, 0.5 parts of modified white graphite are weighed by weight The olefin powder, 30 parts of light calcium carbonate and 1 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 °
  • Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C to further Sealing effect.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of Vaseline, 3 parts of silane coupling agent KH-550, 1 part of modified white graphite are weighed according to the parts by weight The olefin powder, 25 parts of light calcium carbonate and 1.5 parts of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the hollow glass is modified.
  • White graphene composite butyl sealant 10 parts of coumarone resin, 5 parts of Vaseline, 3 parts of silane coupling agent KH-550, 1 part of modified white graphite are weighed according to the parts by weight The olefin powder, 25 parts of light calcium carbonate and 1.5 parts of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing
  • Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass by a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C. Further sealing effect.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2 Kneading of the base rubber component: 40 parts of butyl rubber and 60 parts of polyisobutylene are weighed and mixed in a vacuum kneader, and kneaded at 140 ° C for 60 min to obtain a uniform base rubber component. ;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of petrolatum, 1 part of silane coupling agent KH-570, 0.1 part of modified white graphene powder are weighed by weight 40 parts of carbon black and 0.5 part of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl glass is obtained.
  • Base sealant 10 parts of rosin, 5 parts of petrolatum, 1 part of silane coupling agent KH-570, 0.1 part of modified white graphene powder are weighed by weight 40 parts of carbon black and 0.5 part of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite but
  • Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2) kneading of the base rubber 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are weighed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-570, and 0.5 parts of modified white graphene powder are weighed by weight 30 parts of carbon black and 1 part of antioxidant NBC are added to the vacuum kneader of step 2) and mixed and stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl for hollow glass is obtained.
  • Base sealant 10 parts of rosin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-570, and 0.5 parts of modified white graphene powder are weighed by weight 30 parts of carbon black and 1 part of antioxidant NBC are added to the vacuum kneader of step 2) and mixed and stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl for hollow glass is obtained.
  • Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
  • Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
  • Step 2) kneading of the base rubber 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are weighed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
  • Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of petrolatum, 3 parts of silane coupling agent KH-570, and 1 part of modified white graphene powder are weighed by weight 25 parts of carbon black and 1.5 parts of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl glass is obtained.
  • Base sealant 10 parts of rosin, 5 parts of petrolatum, 3 parts of silane coupling agent KH-570, and 1 part of modified white graphene powder are weighed by weight 25 parts of carbon black and 1.5 parts of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl
  • Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
  • Step 1) kneading of the base rubber 50 parts of butyl rubber and 50 parts of polyisobutylene are respectively weighed and mixed in a vacuum kneader, and kneaded at 110 ° C for 120 minutes to obtain a uniform base rubber component;
  • Step 2) Preparation of butyl sealant: Weigh 10 parts of coumarone resin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-550, 30 parts of light calcium carbonate and 1 part of antioxidant D according to the parts by weight. Adding to the vacuum kneading machine of step 1), mixing and stirring, maintaining the vacuum degree of 0.09 MPa, and mixing and stirring at 110 ° C for 90 min to obtain a butyl sealant for insulating glass;
  • Step 3) Uniform the insulating glass prepared in step 2) with a butyl sealant through a hot melt extruder It was applied around the edge of the fireproof glass and the extrusion temperature was controlled at 115 °C.
  • Step 1) kneading of the base rubber 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are respectively weighed and mixed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
  • Step 2) Preparation of butyl sealant: Weigh 10 parts of rosin, 5 parts of petrolatum, 1.5 parts of silane coupling agent KH-570, 30 parts of carbon black and 1 part of antioxidant NBC according to the parts by weight, and add to step 1) Mixing and stirring in a vacuum kneader, maintaining a vacuum of 0.09 MPa, and mixing and stirring at 130 ° C for 60 min to obtain a butyl sealant for insulating glass;
  • Step 3) The insulating glass prepared in the step 2) was uniformly coated with a butyl sealant through a hot melt adhesive extruder around the edge of the fireproof glass to control the extrusion temperature to 135 °C.
  • Table 1 shows the performance parameters of each example butyl sealant:
  • the sealing effect of the modified white graphene composite butyl sealant for insulating glass of the present invention can further reduce the gas and water vapor of the butyl sealant for insulating glass compared with the comparative example.
  • the transmittance is effective to improve the bond strength.
  • the invention also prolongs the service life of the fireproof glass, and is very suitable for the operation of the hot melt adhesive extruder, is environmentally friendly, has permanent plasticity and high applicability.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

Disclosed are a modified white graphene-compounded butyl sealant for hollow glass and a sealing method therefor. The modified white graphene-compounded butyl sealant contains: a basic sealant and an auxiliary. The basic sealant comprises, by weight, 20-60 parts of butyl rubber and 30-70 parts of polyisobutylene. The auxiliary comprises, by weight, 5-30 parts of a tackifier, 5-20 parts of a softener, 0.1-10 parts of a silane coupling agent, 0.01-5 parts of modified white graphene, 10-50 parts of a reinforcing filler and 0.01-5 parts of an anti-aging agent. The Mooney viscosity of the butyl rubber is 20-80. The number-average molecular weight of polyisobutylene is 10000-80000. The modified white graphene-compounded butyl sealant is very suitable for operation in hot melt adhesive extruders, is green and environmentally friendly, has permanent plasticity and a higher applicable value and the sealing performance thereof for hollow glass is further enhanced.

Description

中空玻璃用改性白石墨烯复合丁基密封胶及其密封方法Modified white graphene composite butyl sealant for insulating glass and sealing method thereof 技术领域Technical field
本发明涉及密封胶技术领域，具体涉及一种中空玻璃用改性白石墨烯复合丁基密封胶及其密封方法。The invention relates to the technical field of sealant, in particular to a modified white graphene composite butyl sealant for insulating glass and a sealing method thereof.
背景技术Background technique
随着国家对节能材料的日趋重视以及人们环境意识的日益增强，中空玻璃在建材市场上的应用越来越广泛，同时对其质量的要求也就越来越高。中空玻璃密封胶是决定中空玻璃质量性能的主要因素，中空玻璃隔热、隔音、防霜雾性能是通过其内部一层密封、干燥的空气层来实现的。因此，选用中空玻璃密封胶最重要的指标之一是密封材料对气体透过性和水汽透过率的高低。无论是传统的槽铝型中空玻璃还是新型复合胶条中空玻璃，其密封胶的选择和使用是最重要的一个环节。With the increasing emphasis on energy-saving materials in the country and the increasing environmental awareness of people, the application of insulating glass in the building materials market is more and more extensive, and the requirements for its quality are getting higher and higher. Insulating glass sealant is the main factor determining the quality performance of insulating glass. Insulating glass insulation, sound insulation and frost-proof performance are realized by a layer of sealed and dry air inside. Therefore, one of the most important indicators for the selection of insulating glass sealants is the gas permeability and water vapor transmission rate of the sealing material. Whether it is the traditional slotted aluminum hollow glass or the new composite adhesive strip hollow glass, the selection and use of the sealant is the most important link.
目前市场上中空玻璃是通过双道密封来实现的。它的内层密封胶通常采用非硫化的热塑性的丁基密封胶材料，其特点是具有极低的透气率，因而在隔离玻璃内外气体交流时，保持了内部空气的干燥，但其粘合力和强度不能达到所需的要求，也就不能达到完全密封，因此必须由第二道密封材料来保证。市场上普遍采用的是聚硫密封胶或硅酮密封胶作为中空玻璃的第二道密封材料，这种材料既可与内层密封胶有良好的搭配，又可与所接触的玻璃、金属框架有良好的相容性，并且具有一定的强度、弹性以及良好的老化性能。但由于硅酮密封胶的气密性差及聚硫密封胶与玻璃的粘接性不强等缺陷，致使第一道丁基密封胶承受巨大考验，丁基密封胶对气体、水汽透过性如若得不到进一步有效加强，随着时间推移，水汽就容易透过密封胶层向中空玻璃中空层渗透扩散，导致玻璃表面出现结霜发雾现象，影响中空玻璃的使用寿命。 Insulating glass on the market today is achieved by double-pass sealing. Its inner sealant usually uses a non-vulcanized thermoplastic butyl sealant material, which is characterized by extremely low gas permeability, thus maintaining the internal air drying when the gas inside and outside the insulating glass is exchanged, but its adhesion And the strength does not meet the required requirements, and the complete seal cannot be achieved, so it must be guaranteed by the second sealing material. Polysulfide sealant or silicone sealant is commonly used in the market as the second sealing material for insulating glass. This material can be well matched with the inner sealant and the glass and metal frame that is in contact with it. It has good compatibility and has certain strength, elasticity and good aging properties. However, due to the poor airtightness of the silicone sealant and the poor adhesion of the polysulfide sealant to the glass, the first butyl sealant is subjected to a great test, and the butyl sealant has a gas and water vapor permeability. Without further strengthening, over time, water vapor easily penetrates into the hollow layer of the hollow glass through the sealant layer, causing frost and fog on the surface of the glass, which affects the service life of the insulating glass.
发明内容Summary of the invention
有鉴于此，有必要针对上述问题，提供一种中空玻璃用改性白石墨烯复合丁基密封胶及其密封方法。In view of the above, it is necessary to provide a modified white graphene composite butyl sealant for insulating glass and a sealing method thereof for the above problems.
为实现上述目的，本发明采取以下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
本发明的中空玻璃用改性白石墨烯复合丁基密封胶，包括：基胶和助剂；The modified white graphene composite butyl sealant for insulating glass of the invention comprises: a base rubber and an auxiliary agent;
所述的基胶包括重量份数为20～60份的丁基橡胶和30-70份的聚异丁烯；The base rubber comprises 20 to 60 parts by weight of butyl rubber and 30 to 70 parts of polyisobutylene;
所述的助剂包括重量份数为：5～30份增粘剂，5～20份软化剂，0.1～10份硅烷偶联剂，0.01～5份改性白石墨烯，10～50份补强填料，0.01～5份防老剂；The auxiliary agent comprises: 5 to 30 parts by weight of a tackifier, 5 to 20 parts of a softener, 0.1 to 10 parts of a silane coupling agent, 0.01 to 5 parts of a modified white graphene, and 10 to 50 parts by weight. Strong filler, 0.01~5 parts anti-aging agent;
所述的丁基橡胶的门尼粘度为20～80，混炼加工效果最优；The montene rubber has a Mooney viscosity of 20 to 80, and the mixing processing effect is optimal;
所述的聚异丁烯数均分子量为10000～80000，中分子量适合于作为密封材料的基体，密封和粘结效果最优。The polyisobutylene has a number average molecular weight of 10,000 to 80,000, and the medium molecular weight is suitable for the substrate as a sealing material, and the sealing and bonding effects are optimal.
作为优选的，所述的基胶包括重量份数为：30～50份丁基橡胶和40～60份聚异丁烯；Preferably, the base rubber comprises: 30 to 50 parts by weight of butyl rubber and 40 to 60 parts of polyisobutylene;
所述的助剂包括重量份数为：5～20份增粘剂，5～10份软化剂，0.5～5份硅烷偶联剂，0.01～2份改性白石墨烯，10～40份补强填料，0.01～3份防老剂。The auxiliary agent comprises: 5 to 20 parts by weight of a tackifier, 5 to 10 parts of a softener, 0.5 to 5 parts of a silane coupling agent, 0.01 to 2 parts of a modified white graphene, and 10 to 40 parts by weight. Strong filler, 0.01 to 3 parts of anti-aging agent.
作为优选的，所述丁基橡胶的门尼粘度选为50；所述聚异丁烯数均分子量为20000。Preferably, the butyl rubber has a Mooney viscosity of 50; and the polyisobutylene has a number average molecular weight of 20,000.
作为优选的，所述增粘剂为古马隆树脂、环氧树脂、松香中的一种；Preferably, the tackifier is one of coumarone resin, epoxy resin, and rosin;
所述软化剂为凡士林；The softener is petrolatum;
所述硅烷偶联剂为KH-550、KH-560、KH-570中的一种；The silane coupling agent is one of KH-550, KH-560, and KH-570;
所述补强填料为滑石粉、轻质碳酸钙、炭黑中的一种；The reinforcing filler is one of talc, light calcium carbonate and carbon black;
所述防老剂为防老剂D、防老剂124、防老剂NBC中的一种。The anti-aging agent is one of the anti-aging agent D, the anti-aging agent 124, and the anti-aging agent NBC.
一种中空玻璃用改性白石墨烯复合丁基密封胶的密封方法，包括：A sealing method for modified white graphene composite butyl sealant for insulating glass, comprising:
步骤1)白石墨烯改性：1-10层的白石墨烯用质量百分含量为0.1％的表面 活性剂浸泡24小时，经离心、真空干燥后得改性白石墨烯粉体；Step 1) White graphene modification: 1-10 layers of white graphene with a surface percentage of 0.1% by mass The active agent is immersed for 24 hours, and the modified white graphene powder is obtained by centrifugation and vacuum drying;
步骤2)基胶的混炼：按重量份数分别称取丁基橡胶和聚异丁烯在真空捏合机中，经90～150℃下混炼30～150min后得到均匀的基胶组份；Step 2) kneading of the base rubber: weighing the butyl rubber and the polyisobutylene in parts by weight in a vacuum kneader, and kneading at 90 to 150 ° C for 30 to 150 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取一定量的增粘剂、软化剂、硅烷偶联剂、改性白石墨烯粉体、补强填料和防老剂加入到混炼后的基胶中，于真空捏合机中混合搅拌，保持真空度为0.09MPa，经90～150℃下混合搅拌30～120min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: weigh a certain amount of tackifier, softener, silane coupling agent, modified white graphene powder, reinforcing filler and The antioxidant is added to the base rubber after mixing, mixed and stirred in a vacuum kneader to maintain a vacuum of 0.09 MPa, and mixed and stirred at 90 to 150 ° C for 30 to 120 minutes to obtain a modified white graphene composite butyl for hollow glass. Base sealant
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为100～150℃，即可达预期的密封效果。Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass by a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to be 100 to 150 ° C. Achieve the desired sealing effect.
作为优选的，步骤1)中所述的表面活性剂为长链路易斯碱、长链路易斯酸、磺酸化物、季胺化物、非离子型表面活性剂。Preferably, the surfactant described in step 1) is a long chain Lewis base, a long chain Lewis acid, a sulfonate, a quaternary amine, a nonionic surfactant.
作为进一步优选的，所述长链路易斯碱为油胺等；所述长链路易斯酸为长链硼烷等；所述磺酸化物为十二烷基苯磺酸钠等；所述季胺化物为溴化十六烷基吡啶等；所述非离子型表面活性剂为聚环氧乙烷烷基醇酰胺等。Further preferably, the long-chain Lewis base is oleylamine or the like; the long-chain Lewis acid is long-chain borane or the like; the sulfonate is sodium dodecylbenzenesulfonate or the like; and the quaternary amination It is cetylpyridinium bromide or the like; the nonionic surfactant is a polyethylene oxide alkyl alcohol amide or the like.
作为优选的，步骤2)中所述基胶组份混炼温度为100～140℃，混炼时间为60～120min；步骤4)中所述热熔胶挤出机挤出温度控制为110～140℃。Preferably, in step 2), the kneading component has a kneading temperature of 100 to 140 ° C, and the kneading time is 60 to 120 min; and in step 4), the hot melt adhesive extruder has an extrusion temperature of 110 to 140 ° C.
与现有技术相比，本发明的有益效果为：Compared with the prior art, the beneficial effects of the present invention are:
选用1～10层改性白石墨烯作为丁基密封胶的改性微粒，片层排列紧凑、均匀，且阻挡片层数目较多，水汽在丁基密封胶中绕行，路径变长，少量添加就能很好的阻挡水汽通过，有效增加丁基胶的气密性；同时少量添加经表面活性剂处理的白石墨烯即可达到与基体良好的润湿性，起到了补强效果，提高了丁基橡胶的粘结强度。 1~10 layers of modified white graphene are selected as the modified particles of butyl sealant. The layers are compact and uniform, and the number of barrier sheets is large. The water vapor circulates in the butyl sealant, and the path becomes long and small. Adding can well block the passage of water vapor, effectively increase the airtightness of butyl rubber; at the same time, adding a small amount of white graphene treated by surfactant can achieve good wettability with the matrix, which can enhance the effect and improve The bond strength of butyl rubber.
本发明进一步增强了中空玻璃用第一道丁基密封胶对气体和水汽的阻隔性能，有效避免了中空玻璃在较长时间使用后出现的结霜发雾现象，延长了中空玻璃的使用寿命，且非常适用于热熔胶挤出机操作，绿色环保，具有永久塑性和较高的适用价值。The invention further enhances the barrier property of the first butyl sealant for insulating glass to gas and water vapor, effectively avoids the frosting and fogging phenomenon of the insulating glass after a long time of use, and prolongs the service life of the insulating glass. It is very suitable for hot melt extruder operation, green, with permanent plasticity and high applicability.
具体实施方式detailed description
为使本发明的目的、技术方案和优点更加清楚，下面将结合本发明实施例，对本发明的技术方案作进一步清楚、完整地描述。需要说明的是，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。In order to make the objects, the technical solutions and the advantages of the present invention more clearly, the technical solutions of the present invention will be further clearly and completely described below in conjunction with the embodiments of the present invention. It should be noted that the described embodiments are only a part of the embodiments of the invention, and not all of the embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative efforts are within the scope of the present invention.
实施例1Example 1
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶的混炼：按重量份数分别称取50份丁基橡胶和50份聚异丁烯在真空捏合机中，经110℃混炼120min后得到均匀的基胶组份；Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份古马隆树脂、5份凡士林、1份硅烷偶联剂KH-550、0.1份改性白石墨烯粉体、40份轻质碳酸钙和0.5份防老剂D加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经110℃下混合搅拌90min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of petrolatum, 1 part of silane coupling agent KH-550, 0.1 part of modified white graphite are weighed by weight The olefin powder, 40 parts of light calcium carbonate and 0.5 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the modified glass is obtained. White graphene composite butyl sealant;
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为110℃，即可达到进一步密封效果。Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C to further Sealing effect.
实施例2 Example 2
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶的混炼：按重量份数分别称取50份丁基橡胶和50份聚异丁烯在真空捏合机中，经110℃混炼120min后得到均匀的基胶组份；Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份古马隆树脂、5份凡士林、1.5份硅烷偶联剂KH-550、0.5份改性白石墨烯粉体、30份轻质碳酸钙和1份防老剂D加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经110℃下混合搅拌90min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-550, 0.5 parts of modified white graphite are weighed by weight The olefin powder, 30 parts of light calcium carbonate and 1 part of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the hollow glass is modified. White graphene composite butyl sealant;
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为110℃，即可达到进一步密封效果。Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C to further Sealing effect.
实施例3Example 3
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶的混炼：按重量份数分别称取50份丁基橡胶和50份聚异丁烯在真空捏合机中，经110℃混炼120min后得到均匀的基胶组份；Step 2) kneading of the base rubber: weighing 50 parts of butyl rubber and 50 parts of polyisobutylene by weight, respectively, in a vacuum kneader, and kneading at 110 ° C for 120 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份古马隆树脂、5份凡士林、3份硅烷偶联剂KH-550、1份改性白石墨烯粉体、25份轻质碳酸钙和1.5份防老剂D加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经110℃下混合搅拌90min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of coumarone resin, 5 parts of Vaseline, 3 parts of silane coupling agent KH-550, 1 part of modified white graphite are weighed according to the parts by weight The olefin powder, 25 parts of light calcium carbonate and 1.5 parts of the antioxidant D are added to the vacuum kneader of the step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 110 ° C for 90 minutes, the hollow glass is modified. White graphene composite butyl sealant;
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为110℃，即可达到 进一步密封效果。Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass by a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 110 ° C. Further sealing effect.
实施例4Example 4
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶组份的混炼：按重量份数分别称取40份丁基橡胶和60份聚异丁烯在真空捏合机中混炼，经140℃混炼60min后得到均匀的基胶组份；Step 2) Kneading of the base rubber component: 40 parts of butyl rubber and 60 parts of polyisobutylene are weighed and mixed in a vacuum kneader, and kneaded at 140 ° C for 60 min to obtain a uniform base rubber component. ;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份松香、5份凡士林、1份硅烷偶联剂KH-570、0.1份改性白石墨烯粉体、40份炭黑和0.5份防老剂NBC加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经130℃下混合搅拌60min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of petrolatum, 1 part of silane coupling agent KH-570, 0.1 part of modified white graphene powder are weighed by weight 40 parts of carbon black and 0.5 part of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl glass is obtained. Base sealant
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为140℃，即可达到进一步密封效果。Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
实施例5Example 5
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶的混炼：按重量份数分别称取40份丁基橡胶和60份聚异丁烯在真空捏合机中，经140℃混炼60min后得到均匀的基胶组份；Step 2) kneading of the base rubber: 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are weighed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份松香、5份凡士林、1.5份硅烷偶联剂KH-570、0.5份改性白石墨烯粉体、30份炭黑和1份防老剂NBC加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经130℃下混合搅拌60min后得到中空玻璃用改性白石墨烯复合丁基密封胶； Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-570, and 0.5 parts of modified white graphene powder are weighed by weight 30 parts of carbon black and 1 part of antioxidant NBC are added to the vacuum kneader of step 2) and mixed and stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl for hollow glass is obtained. Base sealant
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为140℃，即可达到进一步密封效果。Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
实施例6Example 6
步骤1)白石墨烯改性：选用1～10层的白石墨烯，用0.1％油胺水溶液浸泡24小时，经离心、真空干燥后得到白石墨烯改性粉体；Step 1) White graphene modification: 1 to 10 layers of white graphene are selected, soaked in 0.1% aqueous oleylamine solution for 24 hours, and centrifuged and vacuum dried to obtain white graphene modified powder;
步骤2)基胶的混炼：按重量份数分别称取40份丁基橡胶和60份聚异丁烯在真空捏合机中，经140℃混炼60min后得到均匀的基胶组份；Step 2) kneading of the base rubber: 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are weighed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取10份松香、5份凡士林、3份硅烷偶联剂KH-570、1份改性白石墨烯粉体、25份炭黑和1.5份防老剂NBC加入到步骤2)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经130℃下混合搅拌60min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: 10 parts of rosin, 5 parts of petrolatum, 3 parts of silane coupling agent KH-570, and 1 part of modified white graphene powder are weighed by weight 25 parts of carbon black and 1.5 parts of anti-aging agent NBC are added to the vacuum kneader of step 2), and the mixture is stirred to maintain a vacuum of 0.09 MPa. After mixing and stirring at 130 ° C for 60 minutes, a modified white graphene composite butyl glass is obtained. Base sealant
步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为140℃，即可达到进一步密封效果。Step 4) The hollow glass prepared in the step 3) is uniformly coated on the edge of the fireproof glass with a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to 140 ° C to further Sealing effect.
对比例1Comparative example 1
步骤1)基胶的混炼：按重量份数分别称取50份丁基橡胶和50份聚异丁烯在真空捏合机中混炼，经110℃混炼120min后得到均匀的基胶组份；Step 1) kneading of the base rubber: 50 parts of butyl rubber and 50 parts of polyisobutylene are respectively weighed and mixed in a vacuum kneader, and kneaded at 110 ° C for 120 minutes to obtain a uniform base rubber component;
步骤2)丁基密封胶的制备：按重量份数分别称取10份古马隆树脂、5份凡士林、1.5份硅烷偶联剂KH-550、30份轻质碳酸钙和1份防老剂D加入到步骤1)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经110℃下混合搅拌90min后得到中空玻璃用丁基密封胶；Step 2) Preparation of butyl sealant: Weigh 10 parts of coumarone resin, 5 parts of Vaseline, 1.5 parts of silane coupling agent KH-550, 30 parts of light calcium carbonate and 1 part of antioxidant D according to the parts by weight. Adding to the vacuum kneading machine of step 1), mixing and stirring, maintaining the vacuum degree of 0.09 MPa, and mixing and stirring at 110 ° C for 90 min to obtain a butyl sealant for insulating glass;
步骤3)将步骤2)制备的中空玻璃用丁基密封胶通过热熔胶挤出机均匀 涂覆于防火玻璃边缘四周，控制挤出温度为115℃。Step 3) Uniform the insulating glass prepared in step 2) with a butyl sealant through a hot melt extruder It was applied around the edge of the fireproof glass and the extrusion temperature was controlled at 115 °C.
对比例2Comparative example 2
步骤1)基胶的混炼：按重量份数分别称取40份丁基橡胶和60份聚异丁烯在真空捏合机中混炼，经140℃混炼60min后得到均匀的基胶组份；Step 1) kneading of the base rubber: 40 parts by weight of butyl rubber and 60 parts of polyisobutylene are respectively weighed and mixed in a vacuum kneader, and kneaded at 140 ° C for 60 minutes to obtain a uniform base rubber component;
步骤2)丁基密封胶的制备：按重量份数分别称取10份松香、5份凡士林、1.5份硅烷偶联剂KH-570、30份炭黑和1份防老剂NBC加入到步骤1)的真空捏合机中混合搅拌，保持真空度为0.09MPa，经130℃下混合搅拌60min后得到中空玻璃用丁基密封胶；Step 2) Preparation of butyl sealant: Weigh 10 parts of rosin, 5 parts of petrolatum, 1.5 parts of silane coupling agent KH-570, 30 parts of carbon black and 1 part of antioxidant NBC according to the parts by weight, and add to step 1) Mixing and stirring in a vacuum kneader, maintaining a vacuum of 0.09 MPa, and mixing and stirring at 130 ° C for 60 min to obtain a butyl sealant for insulating glass;
步骤3)将步骤2)制备的中空玻璃用丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为135℃。Step 3) The insulating glass prepared in the step 2) was uniformly coated with a butyl sealant through a hot melt adhesive extruder around the edge of the fireproof glass to control the extrusion temperature to 135 °C.
表1中为测定各实施例丁基密封胶的各项性能参数：Table 1 shows the performance parameters of each example butyl sealant:
表1各实施例丁基密封胶的性能参数Table 1 performance parameters of butyl sealant of each example
Figure PCTCN2017098057-appb-000001
Figure PCTCN2017098057-appb-000001
从上表1可知，与对比例相比，本发明的中空玻璃用改性白石墨烯复合丁基密封胶的密封作用，可以进一步降低中空玻璃用丁基密封胶对气体和水蒸汽 的透过率并能有效提高粘结强度。本发明还延长了防火玻璃的使用寿命，而且非常适用于热熔胶挤出机操作，绿色环保，具有永久塑性及较高的适用价值。It can be seen from the above Table 1 that the sealing effect of the modified white graphene composite butyl sealant for insulating glass of the present invention can further reduce the gas and water vapor of the butyl sealant for insulating glass compared with the comparative example. The transmittance is effective to improve the bond strength. The invention also prolongs the service life of the fireproof glass, and is very suitable for the operation of the hot melt adhesive extruder, is environmentally friendly, has permanent plasticity and high applicability.
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。 The above-mentioned embodiments are merely illustrative of several embodiments of the present invention, and the description thereof is more specific and detailed, but is not to be construed as limiting the scope of the invention. It should be noted that a number of variations and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention. Therefore, the scope of the invention should be determined by the appended claims.

Claims (8)

  1. 一种中空玻璃用改性白石墨烯复合丁基密封胶，其特征在于，包括：基胶和助剂；A modified white graphene composite butyl sealant for insulating glass, characterized in that it comprises: a base rubber and an auxiliary agent;
    所述的基胶包括重量份数为20～60份的丁基橡胶和30-70份的聚异丁烯；The base rubber comprises 20 to 60 parts by weight of butyl rubber and 30 to 70 parts of polyisobutylene;
    所述的助剂包括重量份数为：5～30份增粘剂，5～20份软化剂，0.1～10The auxiliary agent comprises: 5 to 30 parts of a tackifier, 5 to 20 parts of a softener, 0.1 to 10 parts by weight.
    份硅烷偶联剂，0.01～5份改性白石墨烯，10～50份补强填料，0.01～5份防老剂；a silane coupling agent, 0.01 to 5 parts of modified white graphene, 10 to 50 parts of reinforcing filler, 0.01 to 5 parts of an antioxidant;
    所述的丁基橡胶的门尼粘度为20～80；The butyl rubber has a Mooney viscosity of 20 to 80;
    所述的聚异丁烯数均分子量为10000～80000。The polyisobutylene has a number average molecular weight of 10,000 to 80,000.
  2. 根据权利要求1所述的中空玻璃用改性白石墨烯复合丁基密封胶，其特征在于，所述的基胶包括重量份数为：30～50份丁基橡胶和40～60份聚异丁烯；The modified white graphene composite butyl sealant for insulating glass according to claim 1, wherein the base rubber comprises 30 parts by weight to 50 parts by weight of butyl rubber and 40 to 60 parts by weight of polyisobutylene. ;
    所述的助剂包括重量份数为：5～20份增粘剂，5～10份软化剂，0.5～5份硅烷偶联剂，0.01～2份改性白石墨烯，10～40份补强填料，0.01～3份防老剂。The auxiliary agent comprises: 5 to 20 parts by weight of a tackifier, 5 to 10 parts of a softener, 0.5 to 5 parts of a silane coupling agent, 0.01 to 2 parts of a modified white graphene, and 10 to 40 parts by weight. Strong filler, 0.01 to 3 parts of anti-aging agent.
  3. 根据权利要求1或2所述的中空玻璃用改性白石墨烯复合丁基密封胶，其特征在于，所述丁基橡胶的门尼粘度选为50；所述聚异丁烯数均分子量为20000。The modified white graphene composite butyl sealant for insulating glass according to claim 1 or 2, wherein the butyl rubber has a Mooney viscosity of 50; and the polyisobutylene has a number average molecular weight of 20,000.
  4. 根据权利要求1或2所述的中空玻璃用改性白石墨烯复合丁基密封胶，其特征在于，所述增粘剂为古马隆树脂、环氧树脂、松香中的一种；The modified white graphene composite butyl sealant for insulating glass according to claim 1 or 2, wherein the tackifier is one of coumarone resin, epoxy resin and rosin;
    所述软化剂为凡士林；The softener is petrolatum;
    所述硅烷偶联剂为KH-550、KH-560、KH-570中的一种；The silane coupling agent is one of KH-550, KH-560, and KH-570;
    所述补强填料为滑石粉、轻质碳酸钙、炭黑中的一种；The reinforcing filler is one of talc, light calcium carbonate and carbon black;
    所述防老剂为防老剂D、防老剂124、防老剂NBC中的一种。The anti-aging agent is one of the anti-aging agent D, the anti-aging agent 124, and the anti-aging agent NBC.
  5. 一种权利要求1或2所述的中空玻璃用改性白石墨烯复合丁基密封胶的 密封方法，其特征在于，包括：步骤1)白石墨烯改性：1-10层的白石墨烯用质量百分含量为0.1％的表面活性剂浸泡24小时，经离心、真空干燥后得改性白石墨烯粉体；A modified white graphene composite butyl sealant for insulating glass according to claim 1 or 2 The sealing method is characterized in that it comprises: step 1) white graphene modification: 1-10 layers of white graphene are soaked with a surfactant having a mass percentage of 0.1% for 24 hours, and then changed after centrifugation and vacuum drying. White graphene powder;
    步骤2)基胶的混炼：按重量份数分别称取丁基橡胶和聚异丁烯在真空捏合机中，经90～150℃下混炼30～150min后得到均匀的基胶组份；Step 2) kneading of the base rubber: weighing the butyl rubber and the polyisobutylene in parts by weight in a vacuum kneader, and kneading at 90 to 150 ° C for 30 to 150 minutes to obtain a uniform base rubber component;
    步骤3)改性白石墨烯复合丁基密封胶的制备：按重量份数分别称取一定量的增粘剂、软化剂、硅烷偶联剂、改性白石墨烯粉体、补强填料和防老剂加入到混炼后的基胶中，于真空捏合机中混合搅拌，保持真空度为0.09MPa，经90～150℃下混合搅拌30～120min后得到中空玻璃用改性白石墨烯复合丁基密封胶；Step 3) Preparation of modified white graphene composite butyl sealant: weigh a certain amount of tackifier, softener, silane coupling agent, modified white graphene powder, reinforcing filler and The antioxidant is added to the base rubber after mixing, mixed and stirred in a vacuum kneader to maintain a vacuum of 0.09 MPa, and mixed and stirred at 90 to 150 ° C for 30 to 120 minutes to obtain a modified white graphene composite butyl for hollow glass. Base sealant
    步骤4)将步骤3)制备的中空玻璃用改性白石墨烯复合丁基密封胶通过热熔胶挤出机均匀涂覆于防火玻璃边缘四周，控制挤出温度为100～150℃，即可达预期的密封效果。Step 4) The hollow glass prepared by the step 3) is uniformly coated on the edge of the fireproof glass by a modified white graphene composite butyl sealant through a hot melt adhesive extruder, and the extrusion temperature is controlled to be 100 to 150 ° C. Achieve the desired sealing effect.
  6. 根据权利要求5所述的中空玻璃用改性白石墨烯复合丁基密封胶的密封方法，其特征在于，步骤1)中所述的表面活性剂为长链路易斯碱、长链路易斯酸、磺酸化物、季胺化物、非离子型表面活性剂。The method for sealing a modified white graphene composite butyl sealant for insulating glass according to claim 5, wherein the surfactant in the step 1) is a long-chain Lewis base, a long-chain Lewis acid, and a sulfonate. Acidate, quaternary amine, nonionic surfactant.
  7. 根据权利要求6所述的中空玻璃用改性白石墨烯复合丁基密封胶的密封方法，其特征在于，所述长链路易斯碱为油胺；所述长链路易斯酸为长链硼烷；所述磺酸化物为十二烷基苯磺酸钠；所述季胺化物为溴化十六烷基吡啶；所述非离子型表面活性剂为聚环氧乙烷烷基醇酰胺。The method for sealing a modified white graphene composite butyl sealant for insulating glass according to claim 6, wherein the long-chain Lewis base is oleylamine; and the long-chain Lewis acid is long-chain borane; The sulfonate is sodium dodecylbenzenesulfonate; the quaternary amine is cetylpyridinium bromide; and the nonionic surfactant is a polyethylene oxide alkyl alcohol amide.
  8. 根据权利要求5所述的中空玻璃用改性白石墨烯复合丁基密封胶的密封方法，其特征在于，步骤2)中所述基胶组份混炼温度为100～140℃，混炼时间为60～120min；步骤4)中所述热熔胶挤出机挤出温度控制为110～140℃。 The method for sealing a modified white graphene composite butyl sealant for insulating glass according to claim 5, wherein the base rubber component in the step 2) is kneaded at a temperature of 100 to 140 ° C, and the mixing time is It is 60-120 min; the extrusion temperature of the hot melt extruder in step 4) is controlled to be 110-140 °C.
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CN113621343A (en) * 2021-08-06 2021-11-09 科建高分子材料（上海）股份有限公司 Silane modified self-adhesive butyl rubber and waterproof roll containing silane self-adhesive butyl rubber
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CN115558465A (en) * 2022-08-31 2023-01-03 河海大学 Natural rosin-based organic-inorganic hybrid sealant and preparation method and application thereof
CN115367743A (en) * 2022-09-05 2022-11-22 安徽大学 Graphene stripping agent, preparation method of graphene, graphene modified rubber and preparation method of graphene modified rubber
CN115367743B (en) * 2022-09-05 2024-02-09 合肥艾克思维新材料科技有限公司 Graphene stripping agent, preparation method of graphene, graphene modified rubber and preparation method of graphene modified rubber
CN116875210A (en) * 2023-06-05 2023-10-13 江西江远材料科技有限公司 Waterproof sealing adhesive tape
CN116875210B (en) * 2023-06-05 2024-06-04 江西江远材料科技有限公司 Waterproof sealing adhesive tape

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