WO2021057132A1 - 一种适用于水泥基层的沥青聚氨酯防水涂料及其制备方法和应用 - Google Patents

一种适用于水泥基层的沥青聚氨酯防水涂料及其制备方法和应用 Download PDF

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WO2021057132A1
WO2021057132A1 PCT/CN2020/097721 CN2020097721W WO2021057132A1 WO 2021057132 A1 WO2021057132 A1 WO 2021057132A1 CN 2020097721 W CN2020097721 W CN 2020097721W WO 2021057132 A1 WO2021057132 A1 WO 2021057132A1
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waterproof coating
polyurethane prepolymer
cement
asphalt
polyurethane
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PCT/CN2020/097721
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English (en)
French (fr)
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李忠人
贺小钢
徐加康
马世界
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江苏凯伦建材股份有限公司
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Publication of WO2021057132A1 publication Critical patent/WO2021057132A1/zh

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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
    • C09D—COATING 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
    • C09D195/00—Coating compositions based on bituminous materials, e.g. asphalt, tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4804—Two or more polyethers of different physical or chemical nature
    • C08G18/4808—Mixtures of two or more polyetherdiols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/4825—Polyethers containing two hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/61—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • E—FIXED CONSTRUCTIONS
    • E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
    • E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
    • E02D31/00—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution
    • E02D31/02—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution against ground humidity or ground water
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62—Insulation or other protection; Elements or use of specified material therefor
    • E04B1/66—Sealings
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
    • E04D11/00—Roof covering, as far as not restricted to features covered by only one of groups E04D1/00 - E04D9/00; Roof covering in ways not provided for by groups E04D1/00 - E04D9/00, e.g. built-up roofs, elevated load-supporting roof coverings
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium

Definitions

  • the invention belongs to the field of building waterproofing, and specifically relates to an asphalt polyurethane waterproof coating suitable for cement base layers, and a preparation method and application thereof.
  • waterproofing membranes have been greatly promoted and used in construction applications. They are mainly used in building walls, roofs, tunnels, highways, etc., to resist external rainwater and groundwater leakage.
  • Rolled flexible building materials as a leak-free connection between the engineering foundation and the building, are the first barrier for the entire project’s waterproofing, and play a vital role in the entire project. It must be strictly in accordance with GB5027-2002 ( roofing Engineering). Quality acceptance specifications) and design regulations and other requirements for construction.
  • the base layer (currently basically a cement base layer) should have a certain strength, and should not be crusted, loose, uneven, and dust and foreign matter on the roof and sub-silo joints must be removed; the base layer is required to be dry, with a moisture content of less than 8%, etc., Generally, the base layer is whitish without obvious water marks, or a 1m ⁇ 1m linoleum is laid flat on a clean flat surface for 3-4 hours. If the color of the base layer covered with linoleum is still the same as the surrounding uncovered parts, there is no obvious watermark, then it contains water. The rate has met the requirements.
  • waterproofing membrane products mainly include bituminous waterproofing membranes and polymer waterproofing membranes.
  • the pretreatment step includes the control of impurities and moisture content.
  • the impurities are easier to clean, but the moisture content is especially difficult to control in real time and accurately when the weather changes rapidly and the air is humid such as rainy days.
  • the asphalt waterproofing membrane The adhesion to the cement base layer needs to be improved.
  • a reactive modified asphalt base treatment agent has been proposed in the prior art, such as Chinese invention patent CN110184017A.
  • Its raw materials include silane-modified polyurethane prepolymer, asphalt, and asphalt compatibilizer. , Silane dewatering agent, catalyst, filler, silane coupling agent, defoamer.
  • this patent can be used to build a primer on a wet base surface, and emphasizes that it can avoid the problem of carbon dioxide bubbles generated by moisture curing in the prior art, thereby ensuring a firm bond, but it is made by directly adding silane to the isocyanate terminal.
  • Silane grafted polyurethane prepolymer Silane grafted polyurethane prepolymer.
  • silane is a conventional silane coupling agent that can react with isocyanate groups.
  • the method used in the preparation method is dropwise addition, which is not conducive to safe production, and also makes the preparation efficiency low, which is not suitable for industrial production; at the same time, its viscosity is relatively large, which is not conducive to on-site construction.
  • the technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide an improved waterproof coating suitable for cement base layer and having a safe and efficient preparation process, which can be directly coated during use On the cement base layer with high water content, it reacts with silicate in the cement after hydrolysis to improve the adhesion on the wet base layer. At the same time, it can also have excellent bonding strength with the asphalt waterproofing membrane, especially It can have a faster surface drying time and moderate viscosity (basically avoid the step of heating before construction), which is conducive to on-site construction.
  • the invention also provides a method for preparing the above-mentioned asphalt polyurethane waterproof coating suitable for cement base layer.
  • the invention also provides a construction method of asphalt waterproof coiled material.
  • An asphalt polyurethane waterproof coating suitable for cement-based layers includes asphalt, compatibilizers, dewatering agents, catalysts, and fillers.
  • the raw materials also include end-capped polyurethane prepolymers.
  • the body is prepared by reacting a compound represented by formula (I) with a polyurethane prepolymer, the blocked polyurethane prepolymer does not contain terminal isocyanate groups, the blocked polyurethane prepolymer, the asphalt and the The feed mass ratio of the compatibilizer is 30-50:40-60:1;
  • R 1 , R 2 , R 3 , and R 4 are each independently selected from a C 1-8 alkyl group, m is 1 or 2, and n is 1, 2, 3 or 4.
  • R 1 , R 2 , R 3 , R 4 , and m and n can make the reaction of the compound represented by formula (I) of the present invention and the polyurethane prepolymer within a controllable range , Neither too fast nor too slow, so that the entire reaction process can be carried out in a safe and controllable condition, which is convenient for industrial use.
  • the end-capped polyurethane prepolymer is fully end-capped, and the feeding amount of the compound represented by formula (I) and the polyurethane pre-polymer is based on the purpose of obtaining a fully end-capped polyurethane prepolymer. Adjustment.
  • the reaction temperature of the reaction between the compound represented by formula (I) and the polyurethane prepolymer is 60-100°C.
  • R 1 , R 2 , R 3 , and R 4 are each independently selected from methyl, ethyl, propyl, isopropyl, n-butyl, isobutyl, tert-butyl Base, -CH 2 CH 2 CH 2 CH 2 CH 3 , -CH(CH 3 )CH 2 CH 2 CH 3 , -CH 2 CH(CH 3 )CH 2 CH 3 , -CH 2 CH 2 CH(CH 3 ) 2 , -CH(C 2 H 5 )CH 2 CH 3 , -C(CH 3 ) 2 CH 2 CH 3 , -CH(CH 3 )CH(CH 3 ) 2 , -CH 2 C(CH 3 ) 3 or Hexyl.
  • R 1 , R 2 , R 3 , and R 4 are each independently selected from methyl, ethyl or propyl.
  • the content of terminal isocyanate groups in the polyurethane prepolymer is 4-10%.
  • the polyurethane prepolymer is made by reacting a polyol with a polyisocyanate, the polyol is a polyether polyol and/or a polyester polyol, and the polyisocyanate is selected from diisocyanates and A combination of one or more of its prepolymer, triisocyanate and its prepolymer.
  • the polyol is a combination of one or more selected from polyether diols, polyether triols and polyester diols, for example including but not limited to polyether diol 2000 , Polyether triol 3050, polyether diol 8000, polyether diol 6000, polyether diol 1000, polyether diol 400, polyether triol 330N, etc.
  • the polyisocyanate includes But not limited to toluene diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), hexamethylene diisocyanate (HDI), Naphthine diisocyanate (NDI) and so on.
  • the raw material further includes a silane coupling agent and/or an antifoaming agent
  • the silane coupling agent is vinyl triethoxy silane, vinyl trimethoxy silane or vinyl tris ( ⁇ -methoxyethoxy) silane
  • the defoamer is a physical defoamer and/or a chemical defoamer
  • the physical defoamer is a polysiloxane defoamer and/or a silicone defoamer
  • the chemical defoaming agent is a combination of one or more selected from calcium oxide, magnesium oxide and calcium hydroxide.
  • in terms of parts by mass in the raw materials, 30-50 parts of capped polyurethane prepolymer, 40-60 parts of asphalt, 1-2 parts of compatibilizer, and 1- 2 parts, 0.1-0.2 parts of catalyst, 0.5-2 parts of filler, and optionally 0.1-0.5 parts of silane coupling agent and 0.1-0.3 parts of defoamer.
  • the asphalt is a combination of one or more selected from Road No. 10, Road No. 70, Road No. 90, Road No. 100, and Road No. 200.
  • the compatibilizer is polyethylene wax and/or polyacetamide wax.
  • the above two compounds have the characteristics of high temperature, low viscosity, and low temperature thixotropy. Through the selection of molecular linkage, they can have both polar groups and non-polar structures. They can be fully dissolved and mutually dissolved in polyurethane and asphalt respectively. .
  • the water scavenger is silane 171.
  • the catalyst is selected from the group consisting of dibutyltin dilaurate, stannous octoate, environmentally friendly non-butyltin catalysts, bismuth carboxylate catalysts, zinc naphthenate, pentamethyldipropylenetriamine , One or more combinations of tetramethylethylenediamine and bismorpholine catalysts.
  • the filler is selected from fumed silica, gypsum whiskers, nano calcium carbonate, nano aluminum nitride, nano boron nitride, nano aluminum borate, heavy calcium, talc, light calcium , Kaolin and wollastonite powder in one or more combinations.
  • a preparation method of the above-mentioned asphalt polyurethane waterproof coating suitable for cement base layer includes the following steps:
  • Preparation of a blocked polyurethane prepolymer first prepare a polyurethane prepolymer, and then mix and react the compound represented by formula (I) with the polyurethane prepolymer to form the blocked polyurethane prepolymer; wherein Control the molar amount of the terminal amino group in the compound represented by formula (I) to be greater than the terminal isocyanate group contained in the polyurethane prepolymer;
  • the construction method includes: first coating the above-mentioned asphalt polyurethane waterproof coating suitable for the cement base layer on the cement base layer. , Forming a waterproof coating, and then covering the asphalt waterproof coiled material on the waterproof coating.
  • the present invention has the following advantages compared with the prior art:
  • the present invention innovatively uses a specific compound of formula (1) to fully end-cap the polyurethane prepolymer.
  • it can make the process of preparing the end-capped polyurethane prepolymer controllable, avoid violent reactions, improve safety, and at the same time
  • waterproof coatings that can be directly coated on the wet cement base layer. After the groups contained in the blocked polyurethane prepolymer are hydrolyzed, they react with the silicate in the cement to improve the adhesion between the waterproof coating and the substrate layer.
  • It can also have excellent bonding strength with the asphalt waterproofing membrane containing the same material, especially it can have a faster surface drying time and moderate viscosity (basically avoid the step of heating before construction), which is conducive to on-site construction .
  • polyether diol 2000, polyether diol 1000, and polyether diol 400 were purchased from Dongda, respectively, toluene diisocyanate was BASF TDI, and diphenylmethane diisocyanate was BASF MDI;
  • R 1 , R 2 , R 3 , and R 4 are all methyl groups, and m and n are all 1;
  • R 1 , R 2 , R 3 , and R 4 are all methyl groups, m is 2 and n is 1;
  • R 1 and R 2 are both methyl, R 3 and R 4 are both ethyl, m is 1, n is 1;
  • R 1 and R 2 are both ethyl, R 3 and R 4 are both methyl, m is 1, and n is 1.
  • This example provides a bituminous polyurethane waterproof coating suitable for cement base layer.
  • its raw materials include: 30 parts of blocked polyurethane prepolymer, 60 parts of road No. 10 asphalt, 1 part of polyethylene wax, and water removal 171 1 part of silane, 0.1 part of dibutyltin dilaurate, 0.5 part of fumed silica, 0.2 part of vinyl triethoxysilane, and 0.1 part of calcium oxide.
  • the preparation method includes the following steps:
  • Dongda Polyether Glycol 2000 50 parts was vacuum dehydrated at 120°C and -0.1MPA to a moisture content of below 0.05%, and then mixed with 10 parts of BASF TDI and reacted at 80°C for 3 hours.
  • the NCO content was measured to be about The reaction is terminated at 4.6%, and 60 parts of polyurethane prepolymer are made;
  • This example provides a bituminous polyurethane waterproof coating suitable for cement base layer.
  • its raw materials include: 40 parts of blocked polyurethane prepolymer, 55 parts of road No. 10 asphalt, 1 part of polyethylene wax, and water removal 171 1 part of silane, 0.2 part of dibutyltin dilaurate, 0.7 part of fumed silica, 0.1 part of vinyl triethoxysilane, and 0.1 part of calcium oxide.
  • the preparation method includes the following steps:
  • Dongda Polyether Glycol 2000 and 25 parts of Dongda Polyether Glycol 1000 were vacuum dehydrated under the conditions of 120°C and -0.1MPA to a moisture content of below 0.05%, and then mixed with 20 parts of BASF TDI. After reacting at 80°C for 3 hours, the reaction was terminated when the measured NCO content was about 5.8%, and 95 parts of polyurethane prepolymer were made;
  • This example provides a bituminous polyurethane waterproof coating suitable for cement base layer.
  • its raw materials include: 50 parts of blocked polyurethane prepolymer, 40 parts of road No. 10 asphalt, 1 part of polyethylene wax, and water removal 171 1 part of silane, 0.1 part of dibutyltin dilaurate, 0.8 part of fumed silica, 0.2 part of vinyl triethoxysilane, and 0.2 part of calcium oxide.
  • the preparation method includes the following steps:
  • This example provides a bituminous polyurethane waterproof coating suitable for cement base layer.
  • its raw materials include: 50 parts of blocked polyurethane prepolymer, 50 parts of road No. 70 asphalt, 1 part of polyacetamide wax, and 171 1 part of aqueous silane, 0.1 part of dibutyltin dilaurate, 0.8 part of fumed silica, 0.1 part of vinyl triethoxysilane, and 0.2 part of calcium oxide.
  • the preparation method includes the following steps:
  • Example 2 It is basically the same as Example 1, except that: the compound represented by formula (I-1) is replaced with the same molar amount of silane coupling agent, such as aminotriethoxysilane.
  • silane coupling agent such as aminotriethoxysilane.
  • the silane coupling agent is added dropwise to the polyurethane prepolymer for reaction during the preparation of the blocked polyurethane prepolymer in the preparation method.
  • Example 2 It is basically the same as Example 1, except that the polyurethane prepolymer is not subjected to end-capping modification, and the same amount of the prepared polyurethane prepolymer is directly used.

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Abstract

一种适用于水泥基层的沥青聚氨酯防水涂料及其制备方法和应用，其原料包括沥青、相容剂、除水剂、催化剂、填料、封端型聚氨酯预聚体，封端型聚氨酯预聚体由式(Ⅰ)所示化合物与聚氨酯预聚体反应制得，封端型聚氨酯预聚体中不含端异氰酸酯基；制备：先制备封端型聚氨酯预聚体，再与剩余原料混合制成；及上述防水涂料在沥青防水卷材施工于水泥基层上的应用；该制备过程安全，使用时可直接将其涂覆在含水较多的水泥基层上，水解后与水泥中的硅酸盐反应，提升在潮湿基层上的粘接力，还能与沥青防水卷材之间具有极佳的粘接强度，尤其具有较快的表干实干时间、粘度适中，可以避免施工前升温的步骤，有利于现场施工。

Description

一种适用于水泥基层的沥青聚氨酯防水涂料及其制备方法和应用 技术领域
本发明属于建筑防水领域，具体涉及一种适用于水泥基层的沥青聚氨酯防水涂料及其制备方法和应用。
背景技术
目前，防水卷材在施工应用中得到了极大地推广和使用，其主要是用于建筑墙体、屋面、以及隧道、公路等处，起到抵御外界雨水、地下水渗漏的一种可卷曲成卷状的柔性建材产品，作为工程基础与建筑物之间无渗漏连接，是整个工程防水的第一道屏障，对整个工程起着至关重要的作用，必须严格按照GB5027-2002(屋面工程质量验收规范)及设计规定等要求施工。其中对于基层(目前基本是水泥基层)应有一定的强度，不应起壳、松动、凹凸不平、对屋面及分仓缝的尘土及异物必须清除；基层要求干燥，含水量小于8％等，一般基层发白不带明显水痕或一块1m×1m的油毡平坦铺贴在干净的平层表面3-4h，如覆盖油毡的基层表面颜色仍与周围未覆盖部位一样，无明显水印，则含水率已经达到要求。然而在施工过程中，尤其是遇到梅雨天等天气变化快、空气潮湿的时间段施工，基于上述防水卷材施工且施工效果好则需要严格控制水泥基层的水分含量，将对工程进度造成较明显的影响，不利于缩短工期，降低施工成本。
现有技术中防水卷材产品主要有沥青防水卷材和高分子防水卷材，其中沥青防水卷材的应用范围仍然很广泛，但是将其施加在水泥基才层上还存在需要对水泥基层进行预处理的步骤，此步骤包括杂质以及含水量的控制，杂质较易清扫，但是水分含量尤其遇到梅雨天等天气变化快、空气潮湿的时间段，将难以实时准确控制，同时沥青防水卷材与水泥基层的粘接力还有待提高。
针对上述粘接力的问题，目前现有技术中已经提出了一种反应型改性沥青基层处理剂，例如中国发明专利CN110184017A，其原料包括硅烷改性聚氨酯预聚体，沥青，沥青相容剂，硅烷除水剂，催化剂，填料，硅烷偶联剂，消泡剂。此专利虽然能够在潮湿基面上施工打底，并强调 其能够避免现有技术中湿气固化产生二氧化碳气泡的问题，进而确保粘接牢固，但是其采用硅烷直接滴加至端异氰酸酯制得的硅烷接枝聚氨酯预聚体，此处硅烷为常规的能够与异氰酸酯基反应的硅烷偶联剂，而实际生产中尤其是反应量较大时，其与异氰酸酯基反应太剧烈，反应过程并不可控，因此其制备方法中采用的方式是滴加，既不利于安全化生产，也使得制备效率低下，不适于工业化生产；同时其粘度较大，较为不利于现场施工。
发明内容
有鉴于此，本发明所要解决的技术问题是为了克服现有技术中的不足，提供一种改进的适用于水泥基层且制备过程安全、效率高的防水涂料，使用过程中可以直接将其涂覆在含水量较多的水泥基层上，水解后与水泥中的硅酸盐反应，提升在潮湿基层上的粘接力，同时还能够与沥青防水卷材之间具有极佳的粘接强度，尤其是能够具有较快的表干实干时间、粘度适中(基本可以避免施工前升温的步骤)，有利于现场施工。
本发明同时还提供了一种制备上述适用于水泥基层的沥青聚氨酯防水涂料的方法。
本发明同时又提供了一种沥青防水卷材的施工方法。
为解决以上技术问题，本发明采取的一种技术方案如下：
一种适用于水泥基层的沥青聚氨酯防水涂料，其原料包括沥青、相容剂、除水剂、催化剂和填料，所述原料还包括封端型聚氨酯预聚体，所述封端型聚氨酯预聚体由式(Ⅰ)所示化合物与聚氨酯预聚体反应制得，所述封端型聚氨酯预聚体中不含端异氰酸酯基，所述封端型聚氨酯预聚体、所述沥青和所述相容剂的投料质量比为30-50∶40-60∶1；
Figure PCTCN2020097721-appb-000001
式中，R 1、R 2、R 3、R 4分别独立地选自C 1-8的烷基，m为1或2，n为1、2、3或4。
本发明中，上述对R 1、R 2、R 3、R 4，以及m和n的优选限定，能够使得本发明的式(Ⅰ)所示化合物与聚氨酯预聚体的反应在可控范围内，既不会太快也不会太慢，使得整个反应过程能够在安全、可操控的情况下进行，便于工业化利用。
根据本发明，所述封端型聚氨酯预聚体为全封端，所述式(Ⅰ)所示化合物与所述聚氨酯预聚体的投料量根据以获得全封端型聚氨酯预聚体为目的调整。
根据本发明的一些优选方面，所述式(Ⅰ)所示化合物与所述聚氨酯预聚体反应的反应温度为60-100℃。
根据本发明的一些优选且具体的方面，R 1、R 2、R 3、R 4分别独立地选自甲基、乙基、丙基、异丙基、正丁基、异丁基、叔丁基、-CH 2CH 2CH 2CH 2CH 3、-CH(CH 3)CH 2CH 2CH 3、-CH 2CH(CH 3)CH 2CH 3、-CH 2CH 2CH(CH 3) 2、-CH(C 2H 5)CH 2CH 3、-C(CH 3) 2CH 2CH 3、-CH(CH 3)CH(CH 3) 2、-CH 2C(CH 3) 3或己基。
根据本发明的一个具体方面，R 1、R 2、R 3、R 4分别独立地选自甲基、乙基或丙基。
根据本发明的一些优选方面，所述聚氨酯预聚体中的端异氰酸酯基的含量为4-10％。
根据本发明的一些实施方案，所述聚氨酯预聚体由多元醇与多异氰酸酯反应制成，所述多元醇为聚醚多元醇和/或聚酯多元醇，所述多异氰酸酯为选自二异氰酸酯及其预聚体、三异氰酸酯及其预聚体中的一种或多种的组合。在一些实施方案中，所述多元醇为选自聚醚二元醇、聚醚三元醇和聚酯二元醇中的一种或多种的组合，例如包括但不限于聚醚二元醇2000、聚醚三元醇3050、聚醚二元醇8000、聚醚二元醇6000、聚醚二元醇1000、聚醚二元醇400、聚醚三元醇330N等等，所述多异氰酸酯包括但不限于甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、萘氨酸二异氰酸酯(NDI)等等。
根据本发明的一些优选方面，所述原料还包括硅烷偶联剂和/或消泡剂，所述硅烷偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷或乙烯基三(β-甲氧乙氧基)硅烷；所述消泡剂为物理消泡剂和/或化学消泡剂，所述物理消泡剂为聚硅氧烷消泡剂和/或硅酮消泡剂，所述化学消泡剂为选自氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。在本发明中，在原料中添加硅烷偶联剂能够在一定程度上提升防水涂料与水泥基材层的粘接力。
根据本发明的一些优选方面，以质量份数计，所述原料中，封端型聚氨酯预聚体30-50份、沥青40-60份、相容剂1-2份、除水剂1-2份、催化剂0.1-0.2份、填料0.5-2份，选择性地包括硅烷偶联剂0.1-0.5份、消泡剂0.1-0.3份。
在本发明的一些实施方案中，所述沥青为选自道路10号、道路70号、道路90号、道路100号和道路200号中的一种或多种的组合。
在本发明的一些实施方案中，所述相容剂为聚乙烯蜡和/或聚乙酰胺蜡。上述两种化合物具有高温低粘、低温触变的特性，通过分子连段的选择可以起到既有极性基团，又有非极性结构，可以在聚氨酯和沥青中分别进行充分的溶解互溶。
在本发明的一些实施方案中，所述除水剂为硅烷171。
在本发明的一些实施方案中，所述催化剂为选自二月桂酸二丁基锡、辛酸亚锡、环保非丁基锡催化剂、羧酸铋类催化剂、环烷酸锌、五甲基二亚丙基三胺、四甲基乙二胺和双吗啉类催化剂中的一种或多种的组合。
在本发明的一些实施方案中，所述填料为选自气相二氧化硅、石膏晶须、纳米碳酸钙、纳米氮化铝、纳米氮化硼、纳米硼酸铝、重钙、滑石粉、轻钙、高岭土和硅灰石粉中的一种或多种的组合。
本发明提供的又一技术方案：一种上述所述的适用于水泥基层的沥青聚氨酯防水涂料的制备方法，所述制备方法包括如下步骤：
(1)制备封端型聚氨酯预聚体：首先制备聚氨酯预聚体，然后将式(Ⅰ)所示化合物与聚氨酯预聚体混合，反应，制成所述封端型聚氨 酯预聚体；其中控制式(Ⅰ)所示化合物中的端氨基的摩尔投料量大于所述聚氨酯预聚体中含有的端异氰酸酯基；
(2)制备防水涂料：按配方称取各原料，混合，制成。
本发明提供的又一技术方案：一种沥青防水卷材在水泥基层上的施工方法，所述施工方法包括：首先在水泥基层上涂覆如上述所述的适用于水泥基层的沥青聚氨酯防水涂料，形成防水涂层，然后将沥青防水卷材覆设在所述防水涂层上。
由于以上技术方案的采用，本发明与现有技术相比具有如下优点：
本发明创新地采用特定的式(1)化合物对聚氨酯预聚体进行全封端，一方面能够使得制备封端型聚氨酯预聚体的过程可控，避免了剧烈反应，提升了安全性，同时还赋予了防水涂料能够直接涂覆在潮湿水泥基层上，通过封端型聚氨酯预聚体含有的基团水解后与水泥中硅酸盐反应提升了防水涂料与基材层的粘接力，而且还能够与含有相同材质的沥青防水卷材之间具有极佳的粘接强度，尤其是能够具有较快的表干实干时间、粘度适中(基本可以避免施工前升温的步骤)，有利于现场施工。
具体实施方式
以下结合具体实施例对上述方案做进一步说明；应理解，这些实施例是用于说明本发明的基本原理、主要特征和优点，而本发明不受以下实施例的范围限制；实施例中采用的实施条件可以根据具体要求做进一步调整，未注明的实施条件通常为常规实验中的条件。
下述实施例中，如无特别说明，所有原料均来自于商购或者通过本领域的常规方法制备而得。
下述中，聚醚二元醇2000、聚醚二元醇1000、聚醚二元醇400分别购自东大，甲苯二异氰酸酯为巴斯夫TDI，二苯基甲烷二异氰酸酯为巴斯夫MDI；
下述中采用的式(Ⅰ)所示化合物分别具有如下所示结构，均购自于赢创化学：
Figure PCTCN2020097721-appb-000002
Figure PCTCN2020097721-appb-000003
式(Ⅰ-1)：R 1、R 2、R 3、R 4均为甲基，m、n均为1；
式(Ⅰ-2)：R 1、R 2、R 3、R 4均为甲基，m为2，n为1；
式(Ⅰ-3)：R 1、R 2均为甲基，R 3、R 4均为乙基，m为1，n为1；
式(Ⅰ-4)：R 1、R 2均为乙基，R 3、R 4均为甲基，m为1，n为1。
实施例1
本例提供一种适用于水泥基层的沥青聚氨酯防水涂料，以质量份数计，其原料包括：封端型聚氨酯预聚体30份、道路10号沥青60份、聚乙烯蜡1份、除水剂硅烷171 1份、二月桂酸二丁基锡0.1份、气相二氧化硅0.5份、乙烯基三乙氧基硅烷0.2份、氧化钙0.1份。
制备方法包括如下步骤：
(1)制备封端型聚氨酯预聚体：
将50份东大聚醚二元醇2000于120℃和-0.1MPA条件下真空脱水至水分含量0.05％以下，然后将其与10份巴斯夫TDI混合在80℃下反应3h，测得NCO含量约为4.6％时终止反应，制成聚氨酯预聚体60份；
然后将式(Ⅰ-1)所示化合物20份与按上述方法制备的聚氨酯预聚体60份混合，60℃下反应，制成所述封端型聚氨酯预聚体80份；
(2)制备防水涂料：按配方称取各原料，混合，制成。
实施例2
本例提供一种适用于水泥基层的沥青聚氨酯防水涂料，以质量份数计，其原料包括：封端型聚氨酯预聚体40份、道路10号沥青55份、聚乙烯蜡1份、除水剂硅烷171 1份、二月桂酸二丁基锡0.2份、气相二氧化硅0.7份、乙烯基三乙氧基硅烷0.1份、氧化钙0.1份。
制备方法包括如下步骤：
(1)制备封端型聚氨酯预聚体：
将50份东大聚醚二元醇2000、25份东大聚醚二元醇1000于120℃和-0.1MPA条件下真空脱水至水分含量0.05％以下，然后将其与20份巴斯夫TDI混合在80℃下反应3h，测得NCO含量约为5.8％时终止反应，制成聚氨酯预聚体95份；
然后将式(Ⅰ-2)所示化合物50份与按上述方法制备的聚氨酯预 聚体95份混合，60℃下反应，制成所述封端型聚氨酯预聚体145份；
(2)制备防水涂料：按配方称取各原料，混合，制成。
实施例3
本例提供一种适用于水泥基层的沥青聚氨酯防水涂料，以质量份数计，其原料包括：封端型聚氨酯预聚体50份、道路10号沥青40份、聚乙烯蜡1份、除水剂硅烷171 1份、二月桂酸二丁基锡0.1份、气相二氧化硅0.8份、乙烯基三乙氧基硅烷0.2份、氧化钙0.2份。
制备方法包括如下步骤：
(1)制备封端型聚氨酯预聚体：
将25份东大聚醚二元醇400、25份东大聚醚二元醇1000于120℃和-0.1MPA条件下真空脱水至水分含量0.05％以下，然后将其与45份巴斯夫MDI混合在80℃下反应2h，测得NCO含量约为8.17％时终止反应，制成聚氨酯预聚体95份；
然后将式(Ⅰ-3)所示化合物55份与按上述方法制备的聚氨酯预聚体95份混合，60℃下反应，制成所述封端型聚氨酯预聚体150份；
(2)制备防水涂料：按配方称取各原料，混合，制成。
实施例4
本例提供一种适用于水泥基层的沥青聚氨酯防水涂料，以质量份数计，其原料包括：封端型聚氨酯预聚体50份、道路70号沥青50份、聚乙酰胺蜡1份、除水剂硅烷171 1份、二月桂酸二丁基锡0.1份、气相二氧化硅0.8份、乙烯基三乙氧基硅烷0.1份、氧化钙0.2份。
制备方法包括如下步骤：
(1)制备封端型聚氨酯预聚体：
将92份东大聚醚二元醇2000于120℃和-0.1MPA条件下真空脱水至水分含量0.05％以下，然后将其与17份巴斯夫TDI混合在80℃下反应，测得NCO含量约为4％时终止反应，制成聚氨酯预聚体109份；
然后将式(Ⅰ-4)所示化合物36份与按上述方法制备的聚氨酯预聚体109份混合，60℃下反应，制成所述封端型聚氨酯预聚体145份；
(2)制备防水涂料：按配方称取各原料，混合，制成。
对比例1
基本同实施例1，其区别仅在于：将式(Ⅰ-1)所示化合物替换为同等摩尔量的硅烷偶联剂，例如氨基三乙氧基硅烷。
由于硅烷偶联剂与聚氨酯预聚体反应太剧烈，因此制备方法中制备封端型聚氨酯预聚体时将硅烷偶联剂滴加至聚氨酯预聚体中反应。
对比例2
基本同实施例1，其区别仅在于：不对聚氨酯预聚体进行封端改性，直接使用同等量的制备的聚氨酯预聚体。
性能测试
将上述实施例1-4以及对比例1-2获得的防水涂料成膜后，测试其各项性能，具体参见表1。
表1
Figure PCTCN2020097721-appb-000004
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围，凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。

Claims (18)

  1. 一种适用于水泥基层的沥青聚氨酯防水涂料，其原料包括沥青、相容剂、除水剂、催化剂和填料，其特征在于，所述原料还包括封端型聚氨酯预聚体，所述封端型聚氨酯预聚体由式(Ⅰ)所示化合物与聚氨酯预聚体在60-100℃下反应制得，所述封端型聚氨酯预聚体中不含端异氰酸酯基，所述封端型聚氨酯预聚体、所述沥青和所述相容剂的投料质量比为30-50∶40-60∶1，所述聚氨酯预聚体中的端异氰酸酯基的含量为4-10％；
    Figure PCTCN2020097721-appb-100001
    式中，R 1、R 2、R 3、R 4分别独立地选自C 1-8的烷基，m为1或2，n为1、2、3或4；
    其中，所述聚氨酯预聚体由多元醇与多异氰酸酯反应制成，所述多元醇为聚醚多元醇和/或聚酯多元醇，所述多异氰酸酯为选自二异氰酸酯及其预聚体、三异氰酸酯及其预聚体中的一种或多种的组合；
    所述相容剂为聚乙烯蜡和/或聚乙酰胺蜡；
    所述催化剂为选自二月桂酸二丁基锡、辛酸亚锡、环保非丁基锡催化剂、羧酸铋类催化剂、环烷酸锌、五甲基二亚丙基三胺、四甲基乙二胺和双吗啉类催化剂中的一种或多种的组合；
    所述填料为选自气相二氧化硅、石膏晶须、纳米碳酸钙、纳米氮化铝、纳米氮化硼、纳米硼酸铝、重钙、滑石粉、轻钙、高岭土和硅灰石粉中的一种或多种的组合；
    所述原料还包括硅烷偶联剂和消泡剂，所述硅烷偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷或乙烯基三(β-甲氧乙氧基)硅烷；所述消泡剂为物理消泡剂和/或化学消泡剂，所述物理消泡剂为聚硅氧烷消泡剂和/或硅酮消泡剂，所述化学消泡剂为选自氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。
  2. 根据权利要求1所述的适用于水泥基层的沥青聚氨酯防水涂料， 其特征在于，R 1、R 2、R 3、R 4分别独立地选自甲基、乙基、丙基、异丙基、正丁基、异丁基、叔丁基、-CH 2CH 2CH 2CH 2CH 3、-CH(CH 3)CH 2CH 2CH 3、-CH 2CH(CH 3)CH 2CH 3、-CH 2CH 2CH(CH 3) 2、-CH(C 2H 5)CH 2CH 3、-C(CH 3) 2CH 2CH 3、-CH(CH 3)CH(CH 3) 2、-CH 2C(CH 3) 3或己基。
  3. 根据权利要求1所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述除水剂为硅烷171。
  4. 根据权利要求1所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述沥青为选自道路10号、道路70号、道路90号、道路100号和道路200号中的一种或多种的组合。
  5. 一种适用于水泥基层的沥青聚氨酯防水涂料，其原料包括沥青、相容剂、除水剂、催化剂和填料，其特征在于，所述原料还包括封端型聚氨酯预聚体，所述封端型聚氨酯预聚体由式(Ⅰ)所示化合物与聚氨酯预聚体反应制得，所述封端型聚氨酯预聚体中不含端异氰酸酯基，所述封端型聚氨酯预聚体、所述沥青和所述相容剂的投料质量比为30-50∶40-60∶1；
    Figure PCTCN2020097721-appb-100002
    式中，R 1、R 2、R 3、R 4分别独立地选自C 1-8的烷基，m为1或2，n为1、2、3或4。
  6. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述式(Ⅰ)所示化合物与所述聚氨酯预聚体反应的反应温度为60-100℃。
  7. 根据权利要求5或6所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，R 1、R 2、R 3、R 4分别独立地选自甲基、乙基、丙基、异丙基、正丁基、异丁基、叔丁基、-CH 2CH 2CH 2CH 2CH 3、-CH(CH 3)CH 2CH 2CH 3、-CH 2CH(CH 3)CH 2CH 3、-CH 2CH 2CH(CH 3) 2、 -CH(C 2H 5)CH 2CH 3、-C(CH 3) 2CH 2CH 3、-CH(CH 3)CH(CH 3) 2、-CH 2C(CH 3) 3或己基。
  8. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，R 1、R 2、R 3、R 4分别独立地选自甲基、乙基或丙基。
  9. 根据权利要求5或6所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述聚氨酯预聚体中的端异氰酸酯基的含量为4-10％。
  10. 根据权利要求9所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述聚氨酯预聚体由多元醇与多异氰酸酯反应制成，所述多元醇为聚醚多元醇和/或聚酯多元醇，所述多异氰酸酯为选自二异氰酸酯及其预聚体、三异氰酸酯及其预聚体中的一种或多种的组合。
  11. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述原料还包括硅烷偶联剂和消泡剂，所述硅烷偶联剂为乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷或乙烯基三(β-甲氧乙氧基)硅烷；所述消泡剂为物理消泡剂和/或化学消泡剂，所述物理消泡剂为聚硅氧烷消泡剂和/或硅酮消泡剂，所述化学消泡剂为选自氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。
  12. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，以质量份数计，所述原料中，封端型聚氨酯预聚体30-50份、沥青40-60份、相容剂1-2份、除水剂1-2份、催化剂0.1-0.2份、填料0.5-2份，选择性地包括硅烷偶联剂0.1-0.5份、消泡剂0.1-0.3份。
  13. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述沥青为选自道路10号、道路70号、道路90号、道路100号和道路200号中的一种或多种的组合。
  14. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述相容剂为聚乙烯蜡和/或聚乙酰胺蜡。
  15. 根据权利要求5所述的适用于水泥基层的沥青聚氨酯防水涂料，其特征在于，所述除水剂为硅烷171，所述催化剂为选自二月桂酸二丁基锡、辛酸亚锡、环保非丁基锡催化剂、羧酸铋类催化剂、环烷酸锌、五甲基二亚丙基三胺、四甲基乙二胺和双吗啉类催化剂中的一种或多种 的组合，所述填料为选自气相二氧化硅、石膏晶须、纳米碳酸钙、纳米氮化铝、纳米氮化硼、纳米硼酸铝、重钙、滑石粉、轻钙、高岭土和硅灰石粉中的一种或多种的组合。
  16. 一种权利要求1-15中任一项权利要求所述的适用于水泥基层的沥青聚氨酯防水涂料的制备方法，其特征在于，所述制备方法包括如下步骤：
    (1)制备封端型聚氨酯预聚体：首先制备聚氨酯预聚体，然后将式(Ⅰ)所示化合物与聚氨酯预聚体混合，反应，制成所述封端型聚氨酯预聚体；其中控制式(Ⅰ)所示化合物中的端氨基的摩尔投料量大于所述聚氨酯预聚体中含有的端异氰酸酯基；
    (2)制备防水涂料：按配方称取各原料，混合，制成。
  17. 根据权利要求16所述的适用于水泥基层的沥青聚氨酯防水涂料的制备方法，其特征在于，步骤(1)中，使所述反应在60-100℃下进行。
  18. 一种沥青防水卷材在水泥基层上的施工方法，其特征在于，所述施工方法包括：首先在水泥基层上涂覆如权利要求1-15中任一项权利要求所述的适用于水泥基层的沥青聚氨酯防水涂料，形成防水涂层，然后将沥青防水卷材覆设在所述防水涂层上。
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