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CN116948502A - A silane-modified polyether waterproof coating and its preparation method - Google Patents

A silane-modified polyether waterproof coating and its preparation method Download PDF

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CN116948502A
CN116948502A CN202311026562.9A CN202311026562A CN116948502A CN 116948502 A CN116948502 A CN 116948502A CN 202311026562 A CN202311026562 A CN 202311026562A CN 116948502 A CN116948502 A CN 116948502A
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silane
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modified polyether
antioxidant
polyether
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CN116948502B (en
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李建芝
彭延泽
李学江
彭松涛
李建芳
刘雪培
田继斌
谢彦姣
张晓明
曲学平
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Hebei Yuyang Zeli Waterproof Material 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
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D171/00Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D171/02Polyalkylene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2603Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2606Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2603Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2606Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
    • C08G65/2609Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32Polymers modified by chemical after-treatment
    • C08G65/329Polymers modified by chemical after-treatment with organic compounds
    • C08G65/336Polymers modified by chemical after-treatment with organic compounds containing silicon
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic

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Abstract

The invention relates to the technical field of waterproof paint, and provides silane modified polyether waterproof paint and a preparation method thereof, wherein the silane modified polyether waterproof paint comprises the following components in parts by weight: 100 parts of silane modified polyether, 10-30 parts of filler, 1-3 parts of coupling agent, 0.5-1 part of dimethyl cyclohexylamine, 0.5-1 part of cyclohexene imine and 1-2 parts of antioxidant; the silane modified polyether comprises the following components in parts by weight: 100 parts of butylene oxide, 15-25 parts of pentaerythritol, 10-20 parts of maltotetraose, 5-15 parts of vinyl methyl diethoxy silane and 1-3 parts of catalyst. Through the technical scheme, the problems of poor waterproof property and low strength of the polyether coating in the prior art are solved.

Description

一种硅烷改性聚醚防水涂料及其制备方法A silane-modified polyether waterproof coating and its preparation method

技术领域Technical field

本发明涉及防水涂料技术领域,具体的,涉及一种硅烷改性聚醚防水涂料及其制备方法。The present invention relates to the technical field of waterproof coatings. Specifically, it relates to a silane-modified polyether waterproof coating and a preparation method thereof.

背景技术Background technique

防水涂料是指经固化后能形成具有一定的延伸性、弹塑性、抗裂性、抗渗性及耐候性的防水薄膜,起到防水、防渗和保护作用的一种涂料。防水涂料多用于建筑物屋面、地下室、厨卫间、地下车库、蓄水池等部位,以防止雨水、地下水、工业和民用给排水,以及空气中的湿气、蒸汽等侵入建筑物内。目前市场上使用较多的建筑防水涂料中,以聚氨酯防水涂料、聚合物水泥防水涂料、丙烯酸防水涂料、改性沥青防水涂料为主,但是大多数防水涂料尤其是聚氨酯、沥青类防水涂料含有较多的有害组分,不符合建材环保的发展趋势。Waterproof coating refers to a coating that can form a waterproof film with certain extensibility, elastic plasticity, crack resistance, impermeability and weather resistance after curing, and plays a waterproof, anti-seepage and protective role. Waterproof coatings are mostly used on building roofs, basements, kitchens and bathrooms, underground garages, reservoirs and other parts to prevent rainwater, groundwater, industrial and civil water supply and drainage, as well as moisture and steam in the air from intruding into the building. Among the currently used building waterproof coatings on the market, polyurethane waterproof coatings, polymer cement waterproof coatings, acrylic waterproof coatings, and modified asphalt waterproof coatings are the main ones. However, most waterproof coatings, especially polyurethane and asphalt waterproof coatings, contain relatively large amounts of water. There are many harmful components, which is not in line with the development trend of environmental protection in building materials.

而聚醚类涂料具有低粘度、低毒性、使用安全可靠、加工性良好,并且符合涂料建材环保的发展趋势的优势,具有广阔的应用前景,但其存在低强度,易吸潮,易吸收空气中的水分,影响其性能和使用寿命的缺点,在一定程度上限制了其发展。Polyether coatings have the advantages of low viscosity, low toxicity, safe and reliable use, good processability, and are in line with the development trend of environmentally friendly coatings and building materials. They have broad application prospects. However, they have low strength, are easy to absorb moisture, and are easy to absorb air. The moisture in it affects its performance and service life, which limits its development to a certain extent.

发明内容Contents of the invention

本发明提出一种硅烷改性聚醚防水涂料及其制备方法,解决了相关技术中,聚醚涂料防水性差以及强度低的问题。The invention proposes a silane-modified polyether waterproof coating and a preparation method thereof, which solves the problems of poor waterproofness and low strength of polyether coatings in related technologies.

本发明的技术方案如下:The technical solution of the present invention is as follows:

本发明提出一种硅烷改性聚醚防水涂料,包括以下重量份的组分:硅烷改性聚醚100份、填料10~30份、偶联剂1~3份、二甲基环己胺0.5~1份、环己烯亚胺0.5~1份、抗氧剂1~2份;The invention proposes a silane-modified polyether waterproof coating, which includes the following components by weight: 100 parts of silane-modified polyether, 10 to 30 parts of filler, 1 to 3 parts of coupling agent, and 0.5 parts of dimethylcyclohexylamine. ~1 part, 0.5~1 part of cyclohexenimine, 1~2 parts of antioxidant;

硅烷改性聚醚包括以下重量份的组分:环氧丁烷100份、季戊四醇15~25份、麦芽四糖10~20份、乙烯基甲基二乙氧基硅烷5~15份、催化剂1~3份。Silane modified polyether includes the following components by weight: 100 parts of butylene oxide, 15 to 25 parts of pentaerythritol, 10 to 20 parts of maltotetraose, 5 to 15 parts of vinyl methyl diethoxysilane, and 1 catalyst ~3 servings.

作为进一步的技术方案,所述填料为滑石粉、石英粉和高岭土中的一种或多种。As a further technical solution, the filler is one or more of talc powder, quartz powder and kaolin.

作为进一步的技术方案,所述偶联剂为环氧基硅烷、甲基丙烯酰氧基硅烷、甲氧基硅烷中的一种或多种。As a further technical solution, the coupling agent is one or more of epoxy silane, methacryloxy silane, and methoxy silane.

作为进一步的技术方案,所述抗氧剂为抗氧剂246、抗氧剂1010、抗氧剂168和抗氧剂164中一种或多种。As a further technical solution, the antioxidant is one or more of antioxidant 246, antioxidant 1010, antioxidant 168 and antioxidant 164.

作为进一步的技术方案,所述催化剂为有机胺类催化剂。As a further technical solution, the catalyst is an organic amine catalyst.

作为进一步的技术方案,所述硅烷改性聚醚的制备方法,包括以下步骤:As a further technical solution, the preparation method of the silane-modified polyether includes the following steps:

S1、在氮气氛围下,将环氧丁烷、季戊四醇、麦芽四糖进行搅拌预混合,于120~130℃下脱水干燥100~120min,得到预混物;S1. In a nitrogen atmosphere, stir and premix butylene oxide, pentaerythritol, and maltotetose, and dehydrate and dry at 120~130°C for 100~120 minutes to obtain a premix;

S2、将所述预混物降温至90~100℃,加入催化剂、乙烯基甲基二乙氧基硅烷进行搅拌反应60~150min,降温至80~90℃继续反应60~120min,得到硅烷改性聚醚。S2. Cool the premix to 90~100°C, add catalyst and vinylmethyldiethoxysilane and stir for 60~150min. Cool the premix to 80~90°C and continue the reaction for 60~120min to obtain silane modification. polyether.

本发明还提出了一种硅烷改性聚醚防水涂料的制备方法,包括以下步骤:The invention also proposes a preparation method of silane-modified polyether waterproof coating, which includes the following steps:

A1、将填料、抗氧剂均匀混合,在120℃及真空条件下进行脱水干燥,得到混合物A;A1. Mix the filler and antioxidant evenly, and dehydrate and dry under 120°C and vacuum conditions to obtain mixture A;

A2、在真空条件下,降温至70~80℃,将硅烷改性聚醚与所述混合物A进行混合,再加入二甲基环己胺、环己烯亚胺、偶联剂搅拌均匀,得到硅烷改性聚醚防水涂料。A2. Under vacuum conditions, lower the temperature to 70~80°C, mix the silane-modified polyether and the mixture A, then add dimethylcyclohexylamine, cyclohexenimine, and coupling agent and stir evenly to obtain Silane modified polyether waterproof coating.

作为进一步的技术方案,所述A1中混合时间为30~60min。As a further technical solution, the mixing time in A1 is 30 to 60 minutes.

作为进一步的技术方案,所述A1、A2中真空条件下的真空度均<-0.08Mpa。As a further technical solution, the vacuum degrees in A1 and A2 under vacuum conditions are both <-0.08Mpa.

作为进一步的技术方案,所述A2中混合时间为40~80min,搅拌时间为30~40min。As a further technical solution, the mixing time in A2 is 40 to 80 minutes, and the stirring time is 30 to 40 minutes.

本发明的工作原理及有益效果为:The working principle and beneficial effects of the present invention are:

本发明中,利用乙烯基甲基二乙氧基硅烷进行改性得到了硅烷改性聚醚,再配合二甲基环己胺和环己烯亚胺的协同作用,制备效率提高的同时,最终得到了以Si-O-Si键为网络交联点硅烷改性聚醚防水涂料,其具有防水性能优异、强度高的优势;并且硅烷改性聚醚时采用季戊四醇和麦芽四糖复配,协同作为环氧丁烷的起始剂,配合乙烯基甲基二乙氧基硅烷对其进行硅烷氧基封端后,显著提高了硅烷改性聚醚防水涂料的防水性。In the present invention, vinylmethyldiethoxysilane is used for modification to obtain a silane-modified polyether, and then combined with the synergistic effect of dimethylcyclohexylamine and cyclohexenimine, the preparation efficiency is improved, and finally A silane-modified polyether waterproof coating with Si-O-Si bonds as network cross-linking points was obtained, which has the advantages of excellent waterproof performance and high strength; and the silane-modified polyether is compounded with pentaerythritol and maltotetraose, which has a synergistic effect. As the initiator of butylene oxide, vinylmethyldiethoxysilane is used to seal it with a siloxy group, which significantly improves the waterproofness of the silane-modified polyether waterproof coating.

具体实施方式Detailed ways

下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,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作出创造性劳动前提下所获得的所有其他实施例,都涉及本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts fall within the scope of protection of the present invention.

实施例1Example 1

一种硅烷改性聚醚防水涂料,包括以下重量份的组分:硅烷改性聚醚100份、高岭土10份、环氧基硅烷1份、二甲基环己胺0.5份、环己烯亚胺0.5份、抗氧剂246 1份;A silane-modified polyether waterproof coating includes the following components by weight: 100 parts of silane-modified polyether, 10 parts of kaolin, 1 part of epoxy silane, 0.5 parts of dimethylcyclohexylamine, cyclohexene 0.5 part of amine, 1 part of antioxidant 246;

硅烷改性聚醚包括以下重量份的组分:环氧丁烷100份、季戊四醇15份、麦芽四糖10份、乙烯基甲基二乙氧基硅烷5份、叔丁胺1份。The silane-modified polyether includes the following components by weight: 100 parts of butylene oxide, 15 parts of pentaerythritol, 10 parts of maltotetraose, 5 parts of vinylmethyldiethoxysilane, and 1 part of tert-butylamine.

硅烷改性聚醚的制备方法,包括以下步骤:The preparation method of silane-modified polyether includes the following steps:

S1、在氮气氛围下,将环氧丁烷、季戊四醇、麦芽四糖进行搅拌预混合,于120℃下脱水干燥120min,得到预混物;S1. In a nitrogen atmosphere, stir and premix butylene oxide, pentaerythritol, and maltotetraose, and dehydrate and dry at 120°C for 120 minutes to obtain a premix;

S2、将所述预混物降温至90℃,加入叔丁胺、乙烯基甲基二乙氧基硅烷进行搅拌反应150min,降温至80℃继续反应120min,得到硅烷改性聚醚。S2. Cool the premix to 90°C, add tert-butylamine and vinylmethyldiethoxysilane, stir and react for 150 minutes, lower the temperature to 80°C and continue the reaction for 120 minutes to obtain a silane-modified polyether.

一种硅烷改性聚醚防水涂料的制备方法,包括以下步骤:A preparation method of silane-modified polyether waterproof coating, including the following steps:

A1、将高岭土、抗氧剂246均匀混合30min,在120℃及真空度为-0.09Mpa的真空条件下进行脱水干燥,得到混合物A;A1. Mix kaolin and antioxidant 246 evenly for 30 minutes, dehydrate and dry under vacuum conditions of 120°C and a vacuum degree of -0.09Mpa to obtain mixture A;

A2、在真空度为-0.09Mpa的真空条件下,降温至70℃,将硅烷改性聚醚树脂与所述混合物A进行混合80min,再加入二甲基环己胺、环己烯亚胺、环氧基硅烷搅拌40min,得到硅烷改性聚醚防水涂料。A2. Under vacuum conditions with a vacuum degree of -0.09Mpa, lower the temperature to 70°C, mix the silane-modified polyether resin and the mixture A for 80 minutes, and then add dimethylcyclohexylamine, cyclohexenimine, Stir the epoxy silane for 40 minutes to obtain a silane-modified polyether waterproof coating.

实施例2Example 2

一种硅烷改性聚醚防水涂料,包括以下重量份的组分:硅烷改性聚醚100份、石英粉20份、甲氧基硅烷2份、二甲基环己胺0.75份、环己烯亚胺0.75份、抗氧剂1010 1.5份;A silane-modified polyether waterproof coating includes the following components by weight: 100 parts of silane-modified polyether, 20 parts of quartz powder, 2 parts of methoxysilane, 0.75 parts of dimethylcyclohexylamine, and cyclohexene 0.75 parts of imine, 1.5 parts of antioxidant 1010;

硅烷改性聚醚包括以下重量份的组分:环氧丁烷100份、季戊四醇20份、麦芽四糖15份、乙烯基甲基二乙氧基硅烷10份、二乙胺2份。The silane-modified polyether includes the following components by weight: 100 parts of butylene oxide, 20 parts of pentaerythritol, 15 parts of maltotetraose, 10 parts of vinylmethyldiethoxysilane, and 2 parts of diethylamine.

硅烷改性聚醚的制备方法,包括以下步骤:The preparation method of silane-modified polyether includes the following steps:

S1、在氮气氛围下,将环氧丁烷、季戊四醇、麦芽四糖进行搅拌预混合,于125℃下脱水干燥110min,得到预混物;S1. In a nitrogen atmosphere, stir and premix butylene oxide, pentaerythritol, and maltotetraose, and dehydrate and dry at 125°C for 110 minutes to obtain a premix;

S2、将所述预混物降温至95℃,加入二乙胺、乙烯基甲基二乙氧基硅烷进行搅拌反应100min,降温至85℃继续反应90min,得到硅烷改性聚醚。S2. Cool the premix to 95°C, add diethylamine and vinylmethyldiethoxysilane, stir and react for 100 minutes, lower the temperature to 85°C and continue the reaction for 90 minutes to obtain a silane-modified polyether.

一种硅烷改性聚醚防水涂料的制备方法,包括以下步骤:A preparation method of silane-modified polyether waterproof coating, including the following steps:

A1、将石英粉、抗氧剂1010均匀混合45min,在120℃及真空度为-0.10Mpa的真空条件下进行脱水干燥,得到混合物A;A1. Mix quartz powder and antioxidant 1010 evenly for 45 minutes, and perform dehydration and drying under vacuum conditions of 120°C and a vacuum degree of -0.10Mpa to obtain mixture A;

A2、在真空度为-0.10Mpa的真空条件下,降温至75℃,将硅烷改性聚醚树脂与所述混合物A进行混合60min,再加入二甲基环己胺、环己烯亚胺、甲氧基硅烷搅拌35min,得到硅烷改性聚醚防水涂料。A2. Under vacuum conditions with a vacuum degree of -0.10Mpa, lower the temperature to 75°C, mix the silane-modified polyether resin and the mixture A for 60 minutes, and then add dimethylcyclohexylamine, cyclohexenimine, Stir the methoxysilane for 35 minutes to obtain a silane-modified polyether waterproof coating.

实施例3Example 3

一种硅烷改性聚醚防水涂料,包括以下重量份的组分:硅烷改性聚醚100份、滑石粉30份、甲基丙烯酰氧基硅烷3份、二甲基环己胺1份、环己烯亚胺1份、抗氧剂168 2份;A silane-modified polyether waterproof coating includes the following components by weight: 100 parts of silane-modified polyether, 30 parts of talc, 3 parts of methacryloxysilane, 1 part of dimethylcyclohexylamine, 1 part of cyclohexenimine, 2 parts of antioxidant 168;

硅烷改性聚醚包括以下重量份的组分:环氧丁烷100份、季戊四醇25份、麦芽四糖20份、乙烯基甲基二乙氧基硅烷15份、己二胺3份。The silane-modified polyether includes the following components by weight: 100 parts of butylene oxide, 25 parts of pentaerythritol, 20 parts of maltotetraose, 15 parts of vinylmethyldiethoxysilane, and 3 parts of hexamethylenediamine.

硅烷改性聚醚的制备方法,包括以下步骤:The preparation method of silane-modified polyether includes the following steps:

S1、在氮气氛围下,将环氧丁烷、季戊四醇、麦芽四糖进行搅拌预混合,于130℃下脱水干燥100min,得到预混物;S1. In a nitrogen atmosphere, stir and premix butylene oxide, pentaerythritol, and maltotetraose, and dehydrate and dry at 130°C for 100 minutes to obtain a premix;

S2、将所述预混物降温至100℃,加入己二胺、乙烯基甲基二乙氧基硅烷进行搅拌反应60min,降温至90℃继续反应60min,得到硅烷改性聚醚。S2. Cool the premix to 100°C, add hexamethylenediamine and vinylmethyldiethoxysilane to stir and react for 60 minutes, lower the temperature to 90°C and continue the reaction for 60 minutes to obtain a silane-modified polyether.

一种硅烷改性聚醚防水涂料的制备方法,包括以下步骤:A preparation method of silane-modified polyether waterproof coating, including the following steps:

A1、将滑石粉、抗氧剂168均匀混合60min,在120℃及真空度为-0.09Mpa的真空条件下进行脱水干燥,得到混合物A;A1. Mix talc powder and antioxidant 168 evenly for 60 minutes, and perform dehydration and drying under vacuum conditions of 120°C and a vacuum degree of -0.09Mpa to obtain mixture A;

A2、在真空度为-0.09Mpa的真空条件下,降温至80℃,将硅烷改性聚醚树脂与所述混合物A进行混合40min,再加入二甲基环己胺、环己烯亚胺、甲基丙烯酰氧基硅烷搅拌30min,得到硅烷改性聚醚防水涂料。A2. Under vacuum conditions with a vacuum degree of -0.09Mpa, cool down to 80°C, mix the silane-modified polyether resin and the mixture A for 40 minutes, then add dimethylcyclohexylamine, cyclohexenimine, Methacryloyloxysilane was stirred for 30 minutes to obtain a silane-modified polyether waterproof coating.

对比例1Comparative example 1

本对比例与实施例3的区别仅在于只加入二甲基环己胺2份,不加入环己烯亚胺。The only difference between this comparative example and Example 3 is that only 2 parts of dimethylcyclohexylamine are added and cyclohexenimine is not added.

对比例2Comparative example 2

本对比例与实施例3的区别仅在于只加入环己烯亚胺2份,不加入二甲基环己胺。The only difference between this comparative example and Example 3 is that only 2 parts of cyclohexenimine is added and no dimethylcyclohexylamine is added.

对比例3Comparative example 3

本对比例与实施例3的区别仅在于只加入季戊四醇45份,不加入麦芽四糖。The only difference between this comparative example and Example 3 is that only 45 parts of pentaerythritol are added and maltotetraose is not added.

对比例4Comparative example 4

本对比例与实施例3的区别仅在于只加入麦芽四糖45份,不加入季戊四醇。The only difference between this comparative example and Example 3 is that only 45 parts of maltotetraose is added and pentaerythritol is not added.

对比例5Comparative example 5

本对比例与实施例3的区别仅在于不对聚醚进行硅烷改性,即聚醚由以下方法制备:The only difference between this comparative example and Example 3 is that the polyether is not modified with silane, that is, the polyether is prepared by the following method:

S1、在氮气氛围下,将100份环氧丁烷、25份季戊四醇、20份麦芽四糖进行搅拌预混合,于130℃下脱水干燥100min,得到预混物;S1. Under a nitrogen atmosphere, stir and premix 100 parts of butylene oxide, 25 parts of pentaerythritol, and 20 parts of maltotetraose, and dehydrate and dry at 130°C for 100 minutes to obtain a premix;

S2、将预混物降温至100℃,加入3份己二胺进行搅拌反应60min,降温至90℃继续反应60min,得到聚醚。S2. Cool the premix to 100°C, add 3 parts of hexamethylenediamine, stir and react for 60 minutes, lower the temperature to 90°C and continue the reaction for 60 minutes to obtain polyether.

对比例6Comparative example 6

本对比例与实施例3的区别仅在于将乙烯基甲基二乙氧基硅烷改为r-氨基丙基三乙氧基硅烷。The only difference between this comparative example and Example 3 is that vinylmethyldiethoxysilane was changed to r-aminopropyltriethoxysilane.

按照标准GB/T 16777-2008《建筑防水涂料试验方法》中的涂膜制备和性能测试方法,将实施例1~3和对比例1~6的硅烷改性聚醚防水涂料分别密封放置24h后,涂覆在模具中,制成厚度为1.5mm左右的涂膜,在标准试验条件下静放7d后,测试涂膜的拉伸性能、撕裂强度和不透水性,测得结果如表1所示。According to the coating film preparation and performance testing methods in the standard GB/T 16777-2008 "Test Methods for Building Waterproof Coatings", the silane-modified polyether waterproof coatings of Examples 1 to 3 and Comparative Examples 1 to 6 were sealed and placed for 24 hours respectively. , coated in the mold to make a coating film with a thickness of about 1.5mm. After leaving it for 7 days under standard test conditions, the tensile properties, tear strength and water impermeability of the coating film were tested. The measured results are as shown in Table 1 shown.

表1 硅烷改性聚醚防水涂料的性能测试结果Table 1 Performance test results of silane-modified polyether waterproof coating

通过对比实施例3、对比例5和对比例6的数据发现,利用乙烯基甲基二乙氧基硅烷进行改性得到了硅烷改性聚醚,具有更高的防水性和强度;通过对比实施例3和对比例1~2的数据发现,实施例3中的拉伸强度、撕裂强度和防水性均优于对比例1~2,说明二甲基环己胺和环己烯亚胺具有协同作用,制备效率提高的同时,还使得硅烷改性聚醚防水涂料具有防水性能优异、强度高的优势;通过对比实施例3和对比例3~4的数据发现,硅烷改性聚醚时采用季戊四醇和麦芽四糖复配,实施例3的强度和防水性比对比例3~4更优,说明季戊四醇和麦芽四糖配合得到多官能度的聚醚,再配合乙烯基甲基二乙氧基硅烷对其进行硅烷氧基封端后,显著提高了硅烷改性聚醚防水涂料的防水性和强度。By comparing the data of Example 3, Comparative Example 5 and Comparative Example 6, it was found that vinylmethyldiethoxysilane was used for modification to obtain a silane-modified polyether, which has higher waterproofness and strength; implemented by comparison The data of Example 3 and Comparative Examples 1~2 found that the tensile strength, tear strength and waterproofness in Example 3 were all better than those of Comparative Examples 1~2, indicating that dimethylcyclohexylamine and cyclohexenimine have The synergistic effect not only improves the preparation efficiency, but also makes the silane-modified polyether waterproof coating have the advantages of excellent waterproof performance and high strength; by comparing the data of Example 3 and Comparative Examples 3~4, it is found that when using silane-modified polyether Pentaerythritol and maltotetraose are compounded, and the strength and waterproofness of Example 3 are better than those of Comparative Examples 3 to 4, indicating that pentaerythritol and maltotetraose are combined to obtain a multifunctional polyether, and then combined with vinyl methyl diethoxy After silane is capped with siloxy groups, the waterproofness and strength of the silane-modified polyether waterproof coating are significantly improved.

以上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 are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection scope of the present invention. within.

Claims (10)

1. The silane modified polyether waterproof coating is characterized by comprising the following components in parts by weight: 100 parts of silane modified polyether, 10-30 parts of filler, 1-3 parts of coupling agent, 0.5-1 part of dimethyl cyclohexylamine, 0.5-1 part of cyclohexene imine and 1-2 parts of antioxidant;
the silane modified polyether comprises the following components in parts by weight: 100 parts of butylene oxide, 15-25 parts of pentaerythritol, 10-20 parts of maltotetraose, 5-15 parts of vinyl methyl diethoxy silane and 1-3 parts of catalyst.
2. The silane-modified waterproof polyether coating according to claim 1, wherein the filler is one or more of talcum powder, quartz powder and kaolin.
3. The silane-modified polyether waterproof paint of claim 1, wherein the coupling agent is one or more of epoxy silane, methacryloxy silane and methoxy silane.
4. The silane-modified, polyether water-resistant coating of claim 1, wherein said antioxidant is one or more of antioxidant 246, antioxidant 1010, antioxidant 168 and antioxidant 164.
5. The silane-modified polyether waterproof paint of claim 1, wherein the catalyst is an organic amine catalyst.
6. The silane-modified polyether waterproof paint according to claim 1, wherein the preparation method of the silane-modified polyether comprises the following steps:
s1, stirring and premixing butylene oxide, pentaerythritol and maltotetraose in a nitrogen atmosphere, and dehydrating and drying at 120-130 ℃ for 100-120 min to obtain a premix;
s2, cooling the premix to 90-100 ℃, adding a catalyst and vinyl methyl diethoxy silane, stirring and reacting for 60-150 min, cooling to 80-90 ℃ and continuing to react for 60-120 min to obtain silane modified polyether.
7. The preparation method of the silane modified polyether waterproof coating according to any one of claims 1 to 6, which is characterized by comprising the following steps:
a1, uniformly mixing a filler and an antioxidant, and dehydrating and drying at 120 ℃ under vacuum conditions to obtain a mixture A;
and A2, cooling to 70-80 ℃ under vacuum condition, mixing the silane modified polyether with the mixture A, and then adding the dimethylcyclohexylamine, cyclohexene imine and the coupling agent to stir uniformly to obtain the silane modified polyether waterproof coating.
8. The preparation method of the silane modified polyether waterproof paint according to claim 7, wherein the mixing time in the A1 is 30-60 min.
9. The preparation method of the silane modified polyether waterproof paint according to claim 7, wherein the vacuum degree of the A1 and the A2 under the vacuum condition is less than-0.08 Mpa.
10. The preparation method of the silane modified polyether waterproof coating according to claim 7, wherein the mixing time in the A2 is 40-80 min, and the stirring time is 30-40 min.
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