CN107384303A - Silicone sealant that steam-preventing passes through and preparation method thereof - Google Patents
Silicone sealant that steam-preventing passes through and preparation method thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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
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Abstract
Description
技术领域technical field
本发明属于密封材料技术领域,具体涉及一种防水蒸汽透过的硅酮密封胶及其制备方法。The invention belongs to the technical field of sealing materials, and in particular relates to a waterproof vapor permeable silicone sealant and a preparation method thereof.
背景技术Background technique
硅酮密封胶具有优异的耐气候、湿热、紫外线及其臭氧老化性能,是建筑密封胶首选材料之一。随着建筑幕墙的广泛应用,硅酮密封胶得到了迅猛的发展。干挂石材幕墙迅速兴起,石材已成为高档建筑的外墙装饰主流之一,因此硅酮石材密封胶的应用量逐年增加。Silicone sealant has excellent resistance to weather, heat and humidity, ultraviolet rays and ozone aging performance, and is one of the preferred materials for building sealants. With the wide application of building curtain walls, silicone sealant has been developed rapidly. Dry-hanging stone curtain walls are rising rapidly, and stone has become one of the mainstream decorations for exterior walls of high-end buildings. Therefore, the application of silicone stone sealants is increasing year by year.
中国发明专利申请公开号CN1865383A中公开了一种电子阻燃硅酮密封胶及其制造方法,其阐述了使用氢氧化镁和氢氧化铝代替卤素阻燃剂的优点,但该专利申请方案未涉及水蒸汽透过的问题。申请人还检索了其它相关的专利文献,例如在CN1687288A公开的阻燃性硅酮结构密封胶及其制造方法和CN101368080A提供的膨胀阻燃有机硅密封胶及其制造方法中,均未对提升硅酮密封胶的防水蒸汽透过性能给出技术启示。Chinese Invention Patent Application Publication No. CN1865383A discloses an electronic flame retardant silicone sealant and its manufacturing method, which explains the advantages of using magnesium hydroxide and aluminum hydroxide instead of halogen flame retardants, but the patent application scheme does not involve The problem of water vapor penetration. The applicant has also retrieved other relevant patent documents, for example, in the flame-retardant silicone structural sealant disclosed in CN1687288A and its manufacturing method and the intumescent flame-retardant silicone sealant and its manufacturing method provided by CN101368080A, none of them have improved the silicon The waterproof vapor transmission performance of ketone sealant gives technical inspiration.
发明内容Contents of the invention
本发明提出一种防水蒸汽透过的硅酮密封胶,该密封胶具有良好的阻燃与机械性能,同时能够防止水蒸汽透过。The present invention proposes a silicone sealant that is waterproof and vapor permeable. The sealant has good flame retardancy and mechanical properties, and can prevent water vapor permeation at the same time.
本发明的技术方案是这样实现的:Technical scheme of the present invention is realized like this:
一种防水蒸汽透过的硅酮密封胶,按照重量份数计算,包括以下原料:A silicone sealant for water vapor penetration, calculated in parts by weight, comprising the following raw materials:
α,ω-二羟基聚二甲基硅氧烷80~90份、石油树脂10~20份、二甲基硅油30~50份、阻燃剂20~40份、补强填料20~40份、气相二氧化硅2~6份、交联剂2~5份、偶联剂2~5份及催化剂0.2~1份,所述补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,所述阻燃剂由十溴二苯乙烷与氢氧化铝组成。80-90 parts of α, ω-dihydroxy polydimethylsiloxane, 10-20 parts of petroleum resin, 30-50 parts of dimethyl silicone oil, 20-40 parts of flame retardant, 20-40 parts of reinforcing filler, 2-6 parts of fumed silica, 2-5 parts of cross-linking agent, 2-5 parts of coupling agent and 0.2-1 part of catalyst, the reinforcing filler is composed of nano-cellulose whiskers, zinc oxide whiskers and carbon nano The flame retardant is composed of decabromodiphenylethane and aluminum hydroxide.
优选地,所述纳米纤维素晶须、氧化锌晶须及碳纳米管的质量之比为5~6:3~4:1~3。Preferably, the mass ratio of the nanocellulose whiskers, zinc oxide whiskers and carbon nanotubes is 5-6:3-4:1-3.
优选地,所述交联剂选自甲基三乙酰氧基硅烷、乙烯基三乙酰氧基硅烷和丙基三乙酰氧基硅烷中一种或者两种以上。Preferably, the crosslinking agent is one or more selected from methyltriacetoxysilane, vinyltriacetoxysilane and propyltriacetoxysilane.
优选地,所述偶联剂选自γ-(2,3环氧丙氧)丙基三甲氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷或者γ-氨丙基三乙氧基硅烷。Preferably, the coupling agent is selected from γ-(2,3 glycidoxy)propyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane or γ-aminopropyltriethylsilane Oxysilane.
优选地,所述催化剂为二丁基二月桂酸锡、辛酸亚锡与钛酸异丙酯的混合物。Preferably, the catalyst is a mixture of dibutyltin dilaurate, stannous octoate and isopropyl titanate.
本发明的另一个目的是提供一种防水蒸汽透过的硅酮密封胶的制备方法,包括以下步骤:Another object of the present invention is to provide a method for preparing a waterproof vapor permeable silicone sealant, comprising the following steps:
1)将α,ω-二羟基聚二甲基硅氧烷、石油树脂、催化剂与补强填料加入真空捏合机内,于温度100~160℃,真空度为0.06~0.085MPa,脱水共混60~300分钟,降温至室温得到混合物A;1) Add α, ω-dihydroxypolydimethylsiloxane, petroleum resin, catalyst and reinforcing filler into the vacuum kneader, dehydrate and blend at a temperature of 100-160°C and a vacuum of 0.06-0.085MPa for 60 ~300 minutes, cooled to room temperature to obtain mixture A;
2)将二甲基硅油、阻燃剂、交联剂、气相二氧化硅及偶联剂加入混合物A中搅拌混合,真空度为0.06~0.085MPa,进行化学反应60~120分钟,即得。2) Add simethicone oil, flame retardant, cross-linking agent, fumed silica and coupling agent into mixture A, stir and mix, and carry out chemical reaction for 60-120 minutes at a vacuum degree of 0.06-0.085 MPa to obtain the product.
本发明的有益效果:Beneficial effects of the present invention:
1、本发明采用的补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,其不仅促进其含量更多的补强填料分散在硅橡胶基体中,大大增强其化学反应接触面及活性,提高了产品的拉伸强度与断裂伸长率,耐候性和耐腐蚀性理想,浸水后拉伸强度在2.15~2.34MPa,。该补强填料还与石油树脂协同作用,促进使用树脂在硅橡胶基体分散包裹,降低硅橡胶基体水蒸汽透过率。1. The reinforcing filler used in the present invention is composed of nano-cellulose whiskers, zinc oxide whiskers and carbon nanotubes, which not only promotes the dispersion of reinforcing fillers with more content in the silicone rubber matrix, but also greatly enhances its chemical reaction contact. Surface and activity, improve the tensile strength and elongation at break of the product, ideal weather resistance and corrosion resistance, the tensile strength after immersion in water is 2.15 ~ 2.34MPa. The reinforcing filler also acts synergistically with the petroleum resin to promote the dispersion and wrapping of the resin on the silicone rubber matrix and reduce the water vapor transmission rate of the silicone rubber matrix.
2、本发明采用由十溴二苯乙烷与氢氧化铝组成的阻燃剂,燃烧性能达到FV-0级。2. The present invention uses a flame retardant composed of decabromodiphenylethane and aluminum hydroxide, and its combustion performance reaches FV-0 level.
具体实施方式detailed description
实施例1Example 1
一种防水蒸汽透过的硅酮密封胶,按照重量份数计算,包括以下原料:A silicone sealant for water vapor penetration, calculated in parts by weight, comprising the following raw materials:
α,ω-二羟基聚二甲基硅氧烷86份、石油树脂15份、二甲基硅油40份、阻燃剂31份、补强填料28份、气相二氧化硅4份、甲基三乙酰氧基硅烷3.5份、γ-甲基丙烯酰氧基丙基三甲氧基硅烷3.5份及催化剂0.6份。86 parts of α, ω-dihydroxy polydimethylsiloxane, 15 parts of petroleum resin, 40 parts of dimethyl silicone oil, 31 parts of flame retardant, 28 parts of reinforcing filler, 4 parts of fumed silica, 3.5 parts of acetoxysilane, 3.5 parts of γ-methacryloxypropyltrimethoxysilane, and 0.6 parts of catalyst.
补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,纳米纤维素晶须、氧化锌晶须及碳纳米管的质量之比为5:3:3。阻燃剂由十溴二苯乙烷与氢氧化铝组成。催化剂为二丁基二月桂酸锡、辛酸亚锡与钛酸异丙酯的混合物。The reinforcing filler is composed of nanocellulose whiskers, zinc oxide whiskers and carbon nanotubes, and the mass ratio of nanocellulose whiskers, zinc oxide whiskers and carbon nanotubes is 5:3:3. The flame retardant consists of decabromodiphenylethane and aluminum hydroxide. The catalyst is a mixture of dibutyltin dilaurate, stannous octoate and isopropyl titanate.
制备方法:Preparation:
1)将α,ω-二羟基聚二甲基硅氧烷、石油树脂、催化剂与补强填料加入真空捏合机内,于温度120℃,真空度为0.075MPa,脱水共混100分钟,降温至室温得到混合物A;1) Add α, ω-dihydroxy polydimethylsiloxane, petroleum resin, catalyst and reinforcing filler into a vacuum kneader, dehydrate and blend for 100 minutes at a temperature of 120°C and a vacuum of 0.075MPa, and cool down to Mixture A is obtained at room temperature;
2)将二甲基硅油、阻燃剂、甲基三乙酰氧基硅烷、气相二氧化硅及γ-甲基丙烯酰氧基丙基三甲氧基硅烷加入混合物A中搅拌混合,真空度为0.06MPa,进行化学反应120分钟,即得。2) Add simethicone oil, flame retardant, methyltriacetoxysilane, fumed silica and γ-methacryloxypropyltrimethoxysilane to mixture A and stir to mix, the vacuum degree is 0.06 MPa, carry out chemical reaction for 120 minutes, that is.
实施例2Example 2
一种防水蒸汽透过的硅酮密封胶,按照重量份数计算,包括以下原料:A silicone sealant for water vapor penetration, calculated in parts by weight, comprising the following raw materials:
α,ω-二羟基聚二甲基硅氧烷80份、石油树脂20份、二甲基硅油30份、阻燃剂20份、补强填料20份、气相二氧化硅6份、乙烯基三乙酰氧基硅烷2份、γ-(2,3环氧丙氧)丙基三甲氧基硅烷2份及催化剂0.2份。80 parts of α, ω-dihydroxy polydimethylsiloxane, 20 parts of petroleum resin, 30 parts of dimethyl silicone oil, 20 parts of flame retardant, 20 parts of reinforcing filler, 6 parts of fumed silica, vinyl tri 2 parts of acetoxysilane, 2 parts of γ-(2,3 glycidoxy)propyltrimethoxysilane and 0.2 parts of catalyst.
补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,纳米纤维素晶须、氧化锌晶须及碳纳米管的质量之比为6:3:2。阻燃剂由十溴二苯乙烷与氢氧化铝组成。催化剂为二丁基二月桂酸锡、辛酸亚锡与钛酸异丙酯的混合物。The reinforcing filler is composed of nanocellulose whiskers, zinc oxide whiskers and carbon nanotubes, and the mass ratio of nanocellulose whiskers, zinc oxide whiskers and carbon nanotubes is 6:3:2. The flame retardant consists of decabromodiphenylethane and aluminum hydroxide. The catalyst is a mixture of dibutyltin dilaurate, stannous octoate and isopropyl titanate.
制备方法:Preparation:
1)将α,ω-二羟基聚二甲基硅氧烷、石油树脂、催化剂与补强填料加入真空捏合机内,于温度160℃,真空度为0.06MPa,脱水共混300分钟,降温至室温得到混合物A;1) Add α, ω-dihydroxy polydimethylsiloxane, petroleum resin, catalyst and reinforcing filler into the vacuum kneader, dehydrate and blend for 300 minutes at a temperature of 160°C and a vacuum of 0.06MPa, and cool down to Mixture A is obtained at room temperature;
2)将二甲基硅油、阻燃剂、乙烯基三乙酰氧基硅烷、气相二氧化硅及γ-(2,3环氧丙氧)丙基三甲氧基硅烷加入混合物A中搅拌混合,真空度为0.06MPa,进行化学反应120分钟,即得。2) Add simethicone oil, flame retardant, vinyltriacetoxysilane, fumed silica and γ-(2,3 glycidoxy)propyltrimethoxysilane to mixture A and stir to mix. The density is 0.06MPa, and the chemical reaction is carried out for 120 minutes.
实施例3Example 3
一种防水蒸汽透过的硅酮密封胶,按照重量份数计算,包括以下原料:A silicone sealant for water vapor penetration, calculated in parts by weight, comprising the following raw materials:
α,ω-二羟基聚二甲基硅氧烷90份、石油树脂10份、二甲基硅油50份、阻燃剂40份、补强填料40份、气相二氧化硅2份、丙基三乙酰氧基硅烷5份、γ-氨丙基三乙氧基硅烷5份及催化剂1份。90 parts of α, ω-dihydroxy polydimethylsiloxane, 10 parts of petroleum resin, 50 parts of dimethyl silicone oil, 40 parts of flame retardant, 40 parts of reinforcing filler, 2 parts of fumed silica, propyl trimethicone 5 parts of acetoxysilane, 5 parts of γ-aminopropyltriethoxysilane and 1 part of catalyst.
补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,纳米纤维素晶须、氧化锌晶须及碳纳米管的质量之比为5:4:3。阻燃剂由十溴二苯乙烷与氢氧化铝组成。催化剂为二丁基二月桂酸锡、辛酸亚锡与钛酸异丙酯的混合物。The reinforcing filler is composed of nano-cellulose whiskers, zinc oxide whiskers and carbon nanotubes, and the mass ratio of nano-cellulose whiskers, zinc oxide whiskers and carbon nanotubes is 5:4:3. The flame retardant consists of decabromodiphenylethane and aluminum hydroxide. The catalyst is a mixture of dibutyltin dilaurate, stannous octoate and isopropyl titanate.
制备方法:Preparation:
1)将α,ω-二羟基聚二甲基硅氧烷、石油树脂、催化剂与补强填料加入真空捏合机内,于温度100℃,真空度为0.085MPa,脱水共混60~300分钟,降温至室温得到混合物A;1) Add α, ω-dihydroxy polydimethylsiloxane, petroleum resin, catalyst and reinforcing filler into the vacuum kneader, dehydrate and blend for 60-300 minutes at a temperature of 100°C and a vacuum of 0.085MPa, Cool to room temperature to obtain mixture A;
2)将二甲基硅油、阻燃剂、丙基三乙酰氧基硅烷、气相二氧化硅及γ-氨丙基三乙氧基硅烷加入混合物A中搅拌混合,真空度为0.06~0.085MPa,进行化学反应60~120分钟,即得。2) Add simethicone oil, flame retardant, propyltriacetoxysilane, fumed silica and γ-aminopropyltriethoxysilane to mixture A and stir to mix, the vacuum degree is 0.06-0.085MPa, The chemical reaction is carried out for 60-120 minutes, and the product is obtained.
实施例4Example 4
一种防水蒸汽透过的硅酮密封胶,按照重量份数计算,包括以下原料:A silicone sealant for water vapor penetration, calculated in parts by weight, comprising the following raw materials:
α,ω-二羟基聚二甲基硅氧烷82份、石油树脂15份、二甲基硅油30份、阻燃剂20份、补强填料20份、气相二氧化硅6份、乙烯基三乙酰氧基硅烷2份、γ-(2,3环氧丙氧)丙基三甲氧基硅烷2份及催化剂0.2份。82 parts of α, ω-dihydroxy polydimethylsiloxane, 15 parts of petroleum resin, 30 parts of dimethyl silicone oil, 20 parts of flame retardant, 20 parts of reinforcing filler, 6 parts of fumed silica, vinyl tri 2 parts of acetoxysilane, 2 parts of γ-(2,3 glycidoxy)propyltrimethoxysilane and 0.2 parts of catalyst.
补强填料由纳米纤维素晶须、氧化锌晶须及碳纳米管组成,纳米纤维素晶须、氧化锌晶须及碳纳米管的质量之比为5:4:3。阻燃剂由十溴二苯乙烷与氢氧化铝组成。催化剂为二丁基二月桂酸锡、辛酸亚锡与钛酸异丙酯的混合物。The reinforcing filler is composed of nano-cellulose whiskers, zinc oxide whiskers and carbon nanotubes, and the mass ratio of nano-cellulose whiskers, zinc oxide whiskers and carbon nanotubes is 5:4:3. The flame retardant consists of decabromodiphenylethane and aluminum hydroxide. The catalyst is a mixture of dibutyltin dilaurate, stannous octoate and isopropyl titanate.
制备方法:Preparation:
1)将α,ω-二羟基聚二甲基硅氧烷、石油树脂、催化剂与补强填料加入真空捏合机内,于温度150℃,真空度为0.07MPa,脱水共混200分钟,降温至室温得到混合物A;1) Add α, ω-dihydroxy polydimethylsiloxane, petroleum resin, catalyst and reinforcing filler into the vacuum kneader, dehydrate and blend for 200 minutes at a temperature of 150°C and a vacuum of 0.07MPa, and cool down to Mixture A is obtained at room temperature;
2)将二甲基硅油、阻燃剂、乙烯基三乙酰氧基硅烷、气相二氧化硅及γ-(2,3环氧丙氧)丙基三甲氧基硅烷加入混合物A中搅拌混合,真空度为0.075MPa,进行化学反应80分钟,即得。2) Add simethicone oil, flame retardant, vinyltriacetoxysilane, fumed silica and γ-(2,3 glycidoxy)propyltrimethoxysilane to mixture A and stir to mix. The density is 0.075MPa, and the chemical reaction is carried out for 80 minutes.
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.
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| CN108822791A (en) * | 2018-06-28 | 2018-11-16 | 芜湖市棠华建材科技有限公司 | Flame-proof silicone sealing material and preparation method thereof |
| JP2019533747A (en) * | 2016-10-31 | 2019-11-21 | ワッカー ケミー アクチエンゲゼルシャフトWacker Chemie AG | Single component room temperature curable compositions based on organosilicon compounds and titanium curing catalysts |
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