WO2021022925A1 - 一种单组分耐根穿刺防水涂料及其制备方法 - Google Patents

一种单组分耐根穿刺防水涂料及其制备方法 Download PDF

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WO2021022925A1
WO2021022925A1 PCT/CN2020/097720 CN2020097720W WO2021022925A1 WO 2021022925 A1 WO2021022925 A1 WO 2021022925A1 CN 2020097720 W CN2020097720 W CN 2020097720W WO 2021022925 A1 WO2021022925 A1 WO 2021022925A1
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Prior art keywords
waterproof coating
boron nitride
resistant waterproof
parts
root puncture
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PCT/CN2020/097720
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English (en)
French (fr)
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李忠人
贺小钢
徐加康
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江苏凯伦建材股份有限公司
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Publication of WO2021022925A1 publication Critical patent/WO2021022925A1/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
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/08—Polyurethanes from polyethers
    • 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
    • C09D175/06—Polyurethanes from polyesters
    • 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
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • 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
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron

Definitions

  • the invention belongs to the field of building waterproofing, and specifically relates to a single-component root puncture-resistant waterproof coating and a preparation method thereof.
  • Waterproof coating The coating applied on the base layer is cured to form a waterproof film with a certain strength, good extensibility, crack resistance, impermeability and weather resistance, and also has good temperature adaptability, simple operation and easy maintenance And maintenance. Compared with waterproof coiled material, waterproof coating has strong adaptability to the base layer, and the waterproof layer has no joints and is more reliable. Due to the above characteristics, waterproof coatings are one of the main waterproof materials often used in waterproof engineering.
  • the roof greening system of buildings generally uses ordinary waterproof coatings, either without root puncture resistance, or with root puncture resistance, but with root puncture resistance, its tensile strength, bonding strength, and elongation at break
  • the physical performance and technical indicators, such as the rate, have not reached the desired effect, so the roots of the plants planted in the roof greening will eventually penetrate the waterproof coating layer, resulting in waterproof failure.
  • the current waterproof coatings with root puncture resistance generally use the addition of root inhibitors to achieve root puncture resistance, such as the addition of (R)-2-(4-chloro-2-methylphenoxy) octyl propionate and other root inhibitors,
  • root inhibitors are expensive, difficult to prepare, contain halogen elements, and are not conducive to environmental protection.
  • the technical problem to be solved by the present invention is to overcome the deficiencies in the prior art and provide a single-component waterproof coating that does not add root inhibitors, but also has environmental protection performance and excellent root resistance performance. And it has high strength and good elongation.
  • the invention also provides a method for preparing the above-mentioned single-component waterproof coating.
  • a one-component root puncture-resistant waterproof coating includes polyisocyanates, polyols, chain extenders, and amino latent curing agents.
  • the raw materials also include compounds represented by formula (I) and surface functionalization.
  • Boron nitride, the surface functionalized boron nitride is surface hydroxylated boron nitride and/or surface aminated boron nitride;
  • R 1 is an amino group.
  • R 2 is methyl, ethyl, propyl, -CH 2 -O-CH 3 , -CH 2 CH 2 -O-CH 3 or -CH 2 -O-CH 2 CH 3 .
  • the compound represented by formula (I) is ⁇ -aminopropyltriethoxysilane and/or ⁇ -aminopropyltrimethoxysilane.
  • the surface hydroxylated boron nitride is prepared by mixing boron nitride with an aqueous solution of alkaline hydroxide, and stirring and reacting at a temperature of 90-150°C.
  • the preparation method of the surface hydroxylated boron nitride is specifically as follows: adding boron nitride (purity ⁇ 99%, particle size 2-5 ⁇ m) into a three-necked reaction flask, and then adding In a good sodium hydroxide aqueous solution, mechanically stirred for 10 hours under the heating condition of an oil bath at about 100°C, the resulting mixture is washed with distilled water for many times until the filtrate is neutral, and dried to obtain surface hydroxylated boron nitride.
  • the surface hydroxylated boron nitride can also be obtained commercially.
  • the surface aminated boron nitride is prepared by mixing boron nitride with an amino organic compound, and ball milling under an inert protective gas atmosphere to prepare the aminated boron nitride
  • the amino organic compound is one or more selected from urea, tetraethylenepentamine and triphenylamine.
  • the preparation method of the surface aminated boron nitride is specifically as follows: under a nitrogen atmosphere, add boron nitride and urea in a ball mill, ball mill at room temperature for 10 hours, take out the ball milled mixture, and remove Ionized water is washed for many times, and the surface aminated boron nitride is obtained after drying.
  • the surface aminated boron nitride can also be obtained commercially.
  • the waterproof coating is prepared by the following method: the polyol, polyisocyanate, compound represented by formula (I) and surface functionalized boron nitride are mixed and reacted, and then a chain extender is added to react to prepare a pre
  • the NCO content in the prepolymer obtained after the reaction is controlled to be 2-5%, and the obtained prepolymer is mixed with the remaining raw materials to prepare the waterproof coating.
  • the polyol is at least one selected from the group consisting of polyether diols, polyester diols and polyether triols, for example including but not limited to polyether 330N, polyether 1000, Polyether 2000 and so on.
  • the polyisocyanate is a combination of one or more selected from the group consisting of diisocyanate and its prepolymer, triisocyanate and its prepolymer, for example including but not limited to toluene diisocyanate (TDI ), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), hexamethylene diisocyanate (HDI), naphthyl diisocyanate (NDI) and many more.
  • TDI toluene diisocyanate
  • IPDI isophorone diisocyanate
  • MDI diphenylmethane diisocyanate
  • HMDI dicyclohexylmethane diisocyanate
  • HDI hexamethylene diisocyanate
  • NDI naphthyl diisocyanate
  • 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, A combination of one or more of kaolin and wollastonite powder.
  • the plasticizer is selected from DINP, DIDP, chlorinated paraffin, dioctyl adipate, glycol benzoate, trioctyl phosphate and phenyl alkyl sulfonate. At least one.
  • the antifoaming agent is a polysiloxane antifoaming agent, or a combination of one or more of silicone antifoaming agents, calcium oxide, magnesium oxide, and calcium hydroxide.
  • the catalyst is selected from dibutyl tin dilaurate, stannous octoate, environmentally friendly non-butyl tin catalyst, bismuth carboxylate catalyst, zinc naphthenate, pentamethyldipropylene triamine, At least one of tetramethylethylenediamine and bismorpholines.
  • the chain extender is selected from one or a combination of clearlink 1000, clearlink 3000, jefflink754, jefflink555, jefflink 7027, and jeffamin HK-511.
  • amino-based latent curing agent refers to a latent curing agent capable of hydrolyzing and releasing amino groups.
  • the amino-based latent curing agent is a combination of one or more selected from the group consisting of latent curing agent 401, latent curing agent 402, and latent curing agent 403.
  • a preparation method of the aforementioned single-component root puncture-resistant waterproof coating comprising the following steps:
  • step (2) The dried polyol, surface-functionalized boron nitride, polyisocyanate, and the compound represented by formula (I) obtained in step (1) are mixed and reacted, and then a chain extender is added to react until the NCO content in the reactant reaches the set point Set the value, stop the reaction, and make a prepolymer, the set value is 2-5%;
  • step (3) Mixing the prepolymer obtained in step (2) with the remaining raw materials to prepare the single-component root puncture-resistant waterproof coating.
  • the present invention has the following advantages compared with the prior art:
  • the waterproof coating of the present invention innovatively uses the compound represented by formula (I) and the surface functionalized boron nitride to modify the conventional polyurethane molecular structure, so that the product has a higher hard segment content, greatly improves the tear resistance, and the molecular structure layer by layer It is arranged to form a dense membrane block that is airtight like aluminum foil, which not only achieves excellent root resistance without adding root inhibitors, but also resists the puncture of various developed root plants, has high strength and good elongation, and it also It has strong hydrophobic function (which can further enhance the waterproof effect of the coating, and the water absorption rate is greatly reduced) and thermal conductivity (can conduct heat in time, and boron nitride is white and does not absorb heat easily), and it can be directly on the wet base Application, good adhesion, and excellent acid resistance, alkali resistance and salt resistance, making it especially suitable for roof planting and waterproofing requirements.
  • TDI80 and MDI were purchased from BASF; polyether 330N, polyether 1000, and polyether 2000 were purchased from Bluestar Dongda; clearlink 1000, clearlink 3000, and jefflink754 were purchased from Guangzhou Jianyi; latent curing agent 401 was purchased from Changde Elite .
  • the surface aminated boron nitride used in the following is made by using boron nitride and urea with a feed mass ratio of 1:2, and the details are as follows: under a nitrogen atmosphere, add boron nitride and urea in a ball mill, and at room temperature After ball milling for 10 hours, the mixture after ball milling was taken out, washed with deionized water several times, and dried to obtain surface aminated boron nitride.
  • the surface hydroxylated boron nitride used in the following is made by the following method: add 50g boron nitride (purity ⁇ 99%, particle size 2 ⁇ 5 ⁇ m) into a three-necked reaction flask, and then add the pre-prepared 5mol/L In the sodium hydroxide aqueous solution, mechanically stirred for 10 hours under the heating condition of an oil bath at about 100° C., the resulting mixture was washed with distilled water several times until the filtrate was neutral, and dried to obtain surface hydroxylated boron nitride.
  • This example provides a one-component root puncture-resistant waterproof coating. Its raw materials include: 7 parts of TDI80, 15 parts of polyether 330N, 15 parts of polyether 1000, 0.5 parts of ⁇ -aminopropyltriethoxysilane, surface amination 1 part of boron nitride, 2 parts of clearlink 1000, 3 parts of latent curing agent 401 3 parts of filler (50% of heavy calcium and talc), 15 parts of DINP, 0.1 part of dibutyltin dilaurate.
  • the preparation method includes the following steps: the surface aminated boron nitride, polyether 330N, polyether 1000 are vacuum dehydrated at 120°C and -0.1Mpa until the moisture content is less than 0.05%, and then ⁇ -aminopropyl triethyl is added Silicon oxide and TDI80, react at 80°C for 3h, then add clearlink 1000 for chain extension reaction, react for 1.5h, titrate with NCO to NCO content of 2.5%, stop the reaction, make a prepolymer, then add it to drying for dehydration
  • the filler and the remaining raw materials are mixed to form the single-component root puncture-resistant waterproof coating.
  • This example provides a one-component root puncture-resistant waterproof coating.
  • Its raw materials include: MDI 10 parts, polyether 330N 20 parts, ⁇ -aminopropyl trimethoxysilane 0.5 parts, surface aminated boron nitride 1.5 parts, clearlink 3000 1 part, 401 3.5 parts of latent curing agent, 40 parts of filler (heavy calcium and talc each account for 50%), 10 parts of DINP, 0.5 part of dibutyltin dilaurate.
  • the preparation method includes the following steps: the surface aminated boron nitride and polyether 330N are vacuum dehydrated at 120°C and -0.1Mpa until the moisture content is less than 0.05%, and then ⁇ -aminopropyl trimethoxy silicon and MDI are added , React at 80°C for 3h, then add clearlink 3000 for chain extension reaction, react for 1.5h, titrate with NCO to NCO content of 2.8%, stop the reaction, make a prepolymer, then add the drying and dehydrated filler and the remaining raw materials , Mixed to prepare the single-component root puncture-resistant waterproof coating.
  • This example provides a one-component root puncture-resistant waterproof coating.
  • Its raw materials include: 9 parts of TDI80, 10 parts of polyether 2000, 18 parts of polyether 1000, 0.8 parts of ⁇ -aminopropyltriethoxysilane, and surface hydroxylation 2 parts of boron nitride, 1.5 parts of jefflink754, 401 3 parts of latent curing agent, 35 parts of filler (heavy calcium and talc each account for 50%), 8 parts of DINP, 0.3 parts of dibutyltin dilaurate.
  • the preparation method includes the following steps: dehydrating the surface hydroxylated boron nitride with polyether 2000 and polyether 1000 in vacuum at 120°C and -0.1Mpa until the moisture content is less than 0.05%, and then adding ⁇ -aminopropyl triethyl Silicon oxide and TDI80, react at 80°C for 3h, then add jefflink754 for chain extension reaction, react for 1.5h, titrate with NCO to NCO content of 3.2%, stop the reaction, make prepolymer, then add drying dehydrated The filler and the remaining raw materials are mixed to form the single-component root puncture-resistant waterproof coating.
  • Example 2 It is basically the same as Example 1, except that ⁇ -aminopropyltriethoxysilane is not added and the amount of TDI80 added is adjusted adaptively.
  • Example 2 It is basically the same as in Example 1, except that the surface aminated boron nitride is not added, and the amount of TDI80 added is adjusted adaptively.
  • the enterprise standard root wear resistance method is as follows:
  • the paint root puncture resistance test was carried out in a box, and the waterproof paint prepared in the above-mentioned examples and comparative examples was applied under the plant roots (Pyracantha fortunei). Samples of the test paint are painted in the test chamber.
  • the test box contains a planting soil layer and a dense plant covering layer, which will produce high growth stress from the roots. In order to maintain this high growth stress, appropriate fertilization and watering should be used.
  • the test box is placed in a temperature-controllable greenhouse. Since environmental conditions have an impact on the growth of plants, the growth conditions should be controllable. The experiment period is 1-2 years. After the experiment, the planting soil layer is removed to observe and evaluate whether the test paint has root puncture.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
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  • Inorganic Chemistry (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

一种单组分耐根穿刺防水涂料及其制备方法，其原料包括多异氰酸酯、多元醇、扩链剂、氨基类潜固化剂、式(Ⅰ)所示化合物、表面羟基和/或表面氨基化氮化硼；R 1-(CH 2) n-Si(OR 2) 3(Ⅰ)，R 1为氨基或羟基，R 2为C 1-6烷基或-R 3-O-R 4，R 3、R 4分别独立地选自甲基、乙基或丙基；表面功能化氮化硼、式(Ⅰ)所示化合物的投料量分别占原料总投料量的1-5％、0.5-3％；制备：使多元醇、多异氰酸酯、式(Ⅰ)所示化合物及表面羟基和/或氨基化氮化硼混合反应，再与扩链剂反应制得预聚体，与剩余原料混合制成；在不添加阻根剂的同时还能兼具环保性能和优异的阻根性能，强度高、延伸率好。

Description

一种单组分耐根穿刺防水涂料及其制备方法 技术领域
本发明属于建筑防水领域，具体涉及一种单组分耐根穿刺防水涂料及其制备方法。
背景技术
防水涂料涂抹在基层上的涂料经固化后形成的防水薄膜具有一定的强度，较好的延伸性、抗裂性、抗渗性及耐候性，同时具有良好的温度适应性，操作简便，易于维修与维护。与防水卷材相比，防水涂料对基层的适应性强，并且防水层无接缝，更具可靠性。由于上述特点，防水涂料是防水工程中经常使用的主要防水材料之一。
目前建筑物的屋顶绿化体系一般采用普通的防水涂料，要么没有耐根穿刺性能，要么有耐根穿刺性能，但有耐根穿刺性能的防水涂料，其拉伸强度、粘结强度、断裂伸长率等物理性能技术指标又没有达到理想的效果，从而屋顶绿化种植的植物根系就会最终穿透防水涂料层，导致防水失败。一旦屋面漏水，就将面临将整个屋面铲除、修复并且必将形成高昂的修复重整费用一系列灾难性的问题。同时目前具有耐根穿刺的防水涂料一般采用添加阻根剂来实现耐根穿刺性能，例如添加(R)-2-(4-氯-2-甲基苯氧)丙酸辛酯等阻根剂，然而此类阻根剂成本高、制备困难，含有卤族元素，不利于环保等。
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，提供一种不添加阻根剂的同时还能兼具环保性能和优异的阻根性能的单组分防水涂料，并且强度高、延伸率好。
本发明同时还提供了一种上述单组分防水涂料的制备方法。
为解决以上技术问题，本发明采取的一种技术方案如下：
一种单组分耐根穿刺防水涂料，所述防水涂料的原料包括多异氰酸酯、多元醇、扩链剂、氨基类潜固化剂，所述原料还包括式(Ⅰ)所示化合物、表面功能化氮化硼，所述表面功能化氮化硼为表面羟基化氮化硼和/或表面氨基化氮化硼；
R 1-(CH 2) n-Si(OR 2) 3(Ⅰ)，式中：R 1为氨基或羟基，R 2为C 1-6烷基或-R 3-O-R 4，R 3、R 4分别独立地选自甲基、乙基或丙基；以质量百分含量计，所述表面功能化氮化硼的投料量占所述原料总投料量的1-5％，所述式(Ⅰ)所示化合物的投料量占所述原料总投料量的0.5-3％。
根据本发明的一些优选且具体的方面，R 1为氨基。
根据本发明的一些优选且具体的方面，R 2为甲基、乙基、丙基、-CH 2-O-CH 3、-CH 2CH 2-O-CH 3或-CH 2-O-CH 2CH 3。
根据本发明的一些具体方面，所述式(Ⅰ)所示化合物为γ-氨丙基三乙氧基硅烷和/或γ-氨丙基三甲氧基硅烷。
根据本发明的一些具体且优选的方面，所述表面羟基化氮化硼通过使氮化硼与碱性氢氧化物的水溶液混合，在温度90～150℃下搅拌反应制成。
在本发明的一些实施方式中，所述表面羟基化氮化硼的制备方法具体如下：将氮化硼(纯度≥99％，粒径2～5μm)加入到三口反应瓶中，然后加入事先配制好的氢氧化钠水溶液中，于100℃左右油浴加热条件下机械搅拌10h，所得的混合物经多次用蒸馏水洗涤至滤液为中性，烘干后得到表面羟基化氮化硼。
在本发明的其它实施方式中，所述表面羟基化氮化硼也可以通过商购获得。
根据本发明的一些具体且优选的方面，所述表面氨基化氮化硼通过如下方法制备：使氮化硼与氨基有机化合物混合，在惰性保护气体气氛下球磨制得所述氨基化氮化硼，所述氨基有机化合物为选自尿素、四乙烯五胺和三苯胺中的一种或几种。
在本发明的一些实施方式中，所述表面氨基化氮化硼的制备方法具体如下：在氮气气氛下，在球磨机内加入氮化硼与尿素，在常温下球磨10h，取出球磨后混合物，去离子水洗涤多次，烘干后得到表面氨基化氮化硼。
在本发明的其它实施方式中，所述表面氨基化氮化硼也可以通过商购获得。
根据本发明的一些优选方面，所述防水涂料通过如下方法制备：使多元醇、多异氰酸酯、式(Ⅰ)所示化合物及表面功能化氮化硼混合反应，再加入扩链剂反应制得预聚体，控制反应后所得预聚体中NCO含量为2-5％，将所得预聚体与剩余原料混合制成所述防水涂料。
根据本发明的一些优选方面，以质量份数计，所述原料中，多异氰酸酯5-10份、多元醇20-30份、式(Ⅰ)所示化合物0.5-2份、表面功能化氮化硼0.5-3份、扩链剂1-5份、氨基类潜固化剂1-5份、填料25-45份、增塑剂5-15份、催化剂0.1-1份、消泡剂0-1份。
根据本发明的一些具体方面，所述多元醇为选自聚醚二元醇、聚酯二元醇和聚醚三元醇中的至少一种，例如包括但不限于聚醚330N、聚醚1000、聚醚2000等等。
根据本发明的一些具体方面，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，例如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。
根据本发明的一些具体方面，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。
根据本发明的一些具体方面，所述增塑剂为选自DINP，DIDP、氯化石蜡、己二酸二辛脂、苯甲酸二醇酯、磷酸三辛酯和烷基磺酸苯酯中的至少一种。
根据本发明的一些具体方面，所述消泡剂为聚硅氧烷消泡剂、或硅酮类消泡剂、氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。
根据本发明的一些具体方面，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、双吗啉类中的至少一种。
根据本发明的一些优选方面，所述扩链剂为选自clearlink 1000、clearlink3000、jefflink754、jefflink555、jefflink 7027和jeffamin  HK-511中的一种或者多种的组合。
本发明中“氨基类潜固化剂”即是指能够水解释放出氨基的潜固化剂。根据本发明的一些具体且优选的方面，所述氨基类潜固化剂为选自潜固化剂401、潜固化剂402和潜固化剂403中的一种或多种的组合。
本发明提供的又一技术方案：一种上述所述的单组分耐根穿刺防水涂料的制备方法，所述制备方法包括如下步骤：
(1)在真空条件下将多元醇、表面功能化氮化硼脱水至0.05％以下；
(2)将步骤(1)所得干燥后的多元醇、表面功能化氮化硼以及多异氰酸酯、式(Ⅰ)所示化合物混合反应，然后加入扩链剂反应，直至反应物中NCO含量达到设定值，停止反应，制成预聚体，所述设定值为2-5％；
(3)将步骤(2)所得预聚体与剩余原料混合制成所述单组分耐根穿刺防水涂料。
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：
本发明的防水涂料创新地采用式(Ⅰ)所示化合物及表面功能化氮化硼混合改性常规聚氨酯分子结构，使得产品硬段含量较高、抗撕裂性能大幅度提高，分子结构层层排布形成如铝箔一样不透气的致密膜块，不仅在不添加阻根剂的情况下实现了优异的阻根性能，可抵御各种发达根系植物的穿刺，强度高延伸率好，同时其还具有较强疏水功能(能够进一步增强涂料的防水功效，吸水率大幅度下降)和导热性能(能够及时将热量传导，且氮化硼为白色也不易吸热)，且在潮湿基面上能够直接应用，粘接力好，同时耐酸、耐碱、耐盐性能较为优异，使其尤其适用于屋面的种植及防水要求。
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。TDI80、MDI分别购自巴斯夫；聚醚330N、聚醚1000、聚醚2000分别购自蓝星东大；clearlink 1000、clearlink 3000、jefflink754分别购自广州坚毅；潜固化剂401购自常德艾利特。
下述中采用的表面氨基化氮化硼通过采用投料质量比为1∶2的氮化硼和尿素制成，具体如下：在氮气气氛下，在球磨机内加入氮化硼与尿素，在常温下球磨10h，取出球磨后混合物，去离子水洗涤多次，烘干后得到表面氨基化氮化硼。
下述中采用的表面羟基化氮化硼通过如下方法制成：将50g氮化硼(纯度≥99％，粒径2～5μm)加入到三口反应瓶中，然后加入事先配制好的5mol/L的氢氧化钠水溶液中，于100℃左右油浴加热条件下机械搅拌10h，所得的混合物经多次用蒸馏水洗涤至滤液为中性，烘干后得到表面羟基化氮化硼。
实施例1
本例提供一种单组分耐根穿刺防水涂料，其原料包括：TDI80 7份、聚醚330N 15份、聚醚1000 15份、γ-氨丙基三乙氧基硅烷0.5份、表面氨基化氮化硼1份、clearlink 1000 2份、潜固化剂401 3份、填料30份(重钙、滑石粉各占50％)、DINP 15份、二月桂酸二丁基锡0.1份。
其制备方法包括如下步骤：将表面氨基化氮化硼与聚醚330N、聚醚1000在120℃、-0.1Mpa下真空脱水，直至水分含量低于0.05％，然后加入γ-氨丙基三乙氧基硅和TDI80，在80℃下反应3h，再加入clearlink 1000进行扩链反应，反应1.5h,通过NCO滴定到NCO含量为2.5％，停止反应，制成预聚体，然后加入烘干脱水的填料以及剩余原料，混合制成所述单组分耐根穿刺防水涂料。
实施例2
本例提供一种单组分耐根穿刺防水涂料，其原料包括：MDI 10份、聚醚330N 20份、γ-氨丙基三甲氧基硅烷0.5份、表面氨基化氮化硼1.5份、clearlink 3000 1份、潜固化剂401 3.5份、填料40份(重钙、滑石粉各占50％)、DINP 10份、二月桂酸二丁基锡0.5份。
其制备方法包括如下步骤：将表面氨基化氮化硼与聚醚330N在120℃、-0.1Mpa下真空脱水，直至水分含量低于0.05％，然后加入γ- 氨丙基三甲氧基硅和MDI，在80℃下反应3h，再加入clearlink 3000进行扩链反应，反应1.5h,通过NCO滴定到NCO含量为2.8％，停止反应，制成预聚体，然后加入烘干脱水的填料以及剩余原料，混合制成所述单组分耐根穿刺防水涂料。
实施例3
本例提供一种单组分耐根穿刺防水涂料，其原料包括：TDI80 9份、聚醚2000 10份、聚醚1000 18份、γ-氨丙基三乙氧基硅烷0.8份、表面羟基化氮化硼2份、jefflink754 1.5份、潜固化剂401 3份、填料35份(重钙、滑石粉各占50％)、DINP 8份、二月桂酸二丁基锡0.3份。
其制备方法包括如下步骤：将表面羟基化氮化硼与聚醚2000、聚醚1000在120℃、-0.1Mpa下真空脱水，直至水分含量低于0.05％，然后加入γ-氨丙基三乙氧基硅和TDI80，在80℃下反应3h，再加入jefflink754进行扩链反应，反应1.5h,通过NCO滴定到NCO含量为3.2％，停止反应，制成预聚体，然后加入烘干脱水的填料以及剩余原料，混合制成所述单组分耐根穿刺防水涂料。
对比例1
基本同实施例1，其区别仅在于不添加γ-氨丙基三乙氧基硅烷，适应性调整TDI80的加入量。
对比例2
基本同实施例1，其区别仅在于不添加表面氨基化氮化硼，适应性调整TDI80的加入量。
性能测试
将上述实施例1-3以及对比例1-2所制成的防水涂料进行如下一些性能测试，具体结果参见表1和表2。
表1
Figure PCTCN2020097720-appb-000001
表2
Figure PCTCN2020097720-appb-000002
企业标准耐根穿方法如下：
涂料耐根穿刺试验在箱中进行，并将上述实施例与对比例制备的防水涂料涂覆置于植物根(选用火棘)的下方。试验涂料的试样涂刷在试验箱中。试验箱中包含种植土层和密集的植物覆盖层，这样将产生来自根部的高的生长应力，为了保持这种高的生长应力应适度施肥并浇水灌溉。试验箱安放在可控温的温室里，由于环境条件对植物的生长具有影响，因此，生长条件应具有可控性。以1-2年为实验周期，试验结束后，将种植土层去除，观察并评价试验涂料是否有根穿刺发生。
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 (22)

  1. 一种单组分耐根穿刺防水涂料，所述防水涂料的原料包括多异氰酸酯、多元醇、扩链剂、氨基类潜固化剂，其特征在于，所述原料还包括式(Ⅰ)所示化合物、表面功能化氮化硼，所述表面功能化氮化硼为表面羟基化氮化硼和/或表面氨基化氮化硼；
    R 1-(CH 2) n-Si(OR 2) 3(Ⅰ)，式中：R 1为氨基或羟基，R 2为C 1-6烷基或-R 3-O-R 4，R 3、R 4分别独立地选自甲基、乙基或丙基；以质量百分含量计，所述表面功能化氮化硼的投料量占所述原料总投料量的1-5％，所述式(Ⅰ)所示化合物的投料量占所述原料总投料量的0.5-3％；
    以质量份数计，所述原料中，多异氰酸酯5-10份、多元醇20-30份、式(Ⅰ)所示化合物0.5-2份、表面功能化氮化硼0.5-3份、扩链剂1-5份、氨基类潜固化剂1-5份、填料25-45份、增塑剂5-15份、催化剂0.1-1份、消泡剂0-1份；
    所述防水涂料通过如下方法制备：使多元醇、多异氰酸酯、式(Ⅰ)所示化合物及表面功能化氮化硼混合反应，再加入扩链剂反应制得预聚体，控制反应后所得预聚体中NCO含量为2-5％，将所得预聚体与剩余原料混合制成所述防水涂料。
  2. 根据权利要求1所述的单组分耐根穿刺防水涂料，其特征在于，R 1为氨基。
  3. 根据权利要求1或2所述的单组分耐根穿刺防水涂料，其特征在于，R 2为甲基、乙基、丙基、-CH 2-O-CH 3、-CH 2CH 2-O-CH 3或-CH 2-O-CH 2CH 3。
  4. 根据权利要求3所述的单组分耐根穿刺防水涂料，其特征在于，所述式(Ⅰ)所示化合物为γ-氨丙基三乙氧基硅烷和/或γ-氨丙基三甲氧基硅烷。
  5. 根据权利要求1所述的单组分耐根穿刺防水涂料，其特征在于，所述多元醇为选自聚醚二元醇、聚酯二元醇和聚醚三元醇中的至少一种；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；所述扩链剂为选自clearlink 1000、 clearlink3000、jefflink754、jefflink555、jefflink 7027和jeffamin HK-511中的一种或者多种的组合；所述氨基类潜固化剂为选自潜固化剂401、潜固化剂402和潜固化剂403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；所述增塑剂为选自DINP，DIDP、氯化石蜡、己二酸二辛脂、苯甲酸二醇酯、磷酸三辛酯和烷基磺酸苯酯中的至少一种；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、双吗啉类中的至少一种；所述消泡剂为聚硅氧烷消泡剂、或硅酮类消泡剂、氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。
  6. 一种单组分耐根穿刺防水涂料，所述防水涂料的原料包括多异氰酸酯、多元醇、扩链剂、氨基类潜固化剂，其特征在于，所述原料还包括式(Ⅰ)所示化合物、表面功能化氮化硼，所述表面功能化氮化硼为表面羟基化氮化硼和/或表面氨基化氮化硼；
    R 1-(CH 2) n-Si(OR 2) 3(Ⅰ)，式中：R 1为氨基或羟基，R 2为C 1-6烷基或-R 3-O-R 4，R 3、R 4分别独立地选自甲基、乙基或丙基；以质量百分含量计，所述表面功能化氮化硼的投料量占所述原料总投料量的1-5％，所述式(Ⅰ)所示化合物的投料量占所述原料总投料量的0.5-3％。
  7. 根据权利要求6所述的单组分耐根穿刺防水涂料，其特征在于，R 1为氨基。
  8. 根据权利要求6或7所述的单组分耐根穿刺防水涂料，其特征在于，R 2为甲基、乙基、丙基、-CH 2-O-CH 3、-CH 2CH 2-O-CH 3或-CH 2-O-CH 2CH 3。
  9. 根据权利要求8所述的单组分耐根穿刺防水涂料，其特征在于，所述式(Ⅰ)所示化合物为γ-氨丙基三乙氧基硅烷和/或γ-氨丙基三甲氧基硅烷。
  10. 根据权利要求6所述的单组分耐根穿刺防水涂料，其特征在于，所述表面羟基化氮化硼通过使氮化硼与碱性氢氧化物的水溶液混合，在 温度90～150℃下搅拌反应制成。
  11. 根据权利要求6所述的单组分耐根穿刺防水涂料，其特征在于，所述表面氨基化氮化硼通过如下方法制备：使氮化硼与氨基有机化合物混合，在惰性保护气体气氛下球磨制得所述氨基化氮化硼，所述氨基有机化合物为选自尿素、四乙烯五胺和三苯胺中的一种或几种。
  12. 根据权利要求6所述的单组分耐根穿刺防水涂料，其特征在于，所述防水涂料通过如下方法制备：使多元醇、多异氰酸酯、式(Ⅰ)所示化合物及表面功能化氮化硼混合反应，再加入扩链剂反应制得预聚体，控制反应后所得预聚体中NCO含量为2-5％，将所得预聚体与剩余原料混合制成所述防水涂料。
  13. 根据权利要求6所述的单组分耐根穿刺防水涂料，其特征在于，以质量份数计，所述原料中，多异氰酸酯5-10份、多元醇20-30份、式(Ⅰ)所示化合物0.5-2份、表面功能化氮化硼0.5-3份、扩链剂1-5份、氨基类潜固化剂1-5份、填料25-45份、增塑剂5-15份、催化剂0.1-1份、消泡剂0-1份。
  14. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于，所述多元醇为选自聚醚二元醇、聚酯二元醇和聚醚三元醇中的至少一种。
  15. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于，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。
  16. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于，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。
  17. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于，所述增塑剂为选自DINP，DIDP、氯化石蜡、己二酸二辛脂、苯甲酸二醇酯、磷酸三辛酯和烷基磺酸苯酯中的至少一种。
  18. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于， 所述消泡剂为聚硅氧烷消泡剂、或硅酮类消泡剂、氧化钙、氧化镁和氢氧化钙中的一种或多种的组合。
  19. 根据权利要求13所述的单组分耐根穿刺防水涂料，其特征在于，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、双吗啉类中的至少一种。
  20. 根据权利要求6或13所述的单组分耐根穿刺防水涂料，其特征在于，所述扩链剂为选自clearlink 1000、clearlink3000、jefflink754、jefflink555、jefflink 7027和jeffamin HK-511中的一种或者多种的组合。
  21. 根据权利要求6或13所述的单组分耐根穿刺防水涂料，其特征在于，所述氨基类潜固化剂为选自潜固化剂401、潜固化剂402和潜固化剂403中的一种或多种的组合。
  22. 一种权利要求1-21中任一项权利要求所述的单组分耐根穿刺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)在真空条件下将多元醇、表面功能化氮化硼脱水至0.05％以下；
    (2)将步骤(1)所得干燥后的多元醇、表面功能化氮化硼以及多异氰酸酯、式(Ⅰ)所示化合物混合反应，然后加入扩链剂反应，直至反应物中NCO含量达到设定值，停止反应，制成预聚体，所述设定值为2-5％；
    (3)将步骤(2)所得预聚体与剩余原料混合制成所述单组分耐根穿刺防水涂料。
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