CN114381178A - 一种水性高弹丙烯酸防水涂料及其制备方法 - Google Patents
一种水性高弹丙烯酸防水涂料及其制备方法 Download PDFInfo
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- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B13/00—Preparation of cellulose ether-esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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Abstract
本发明涉及建筑防水材料领域,具体为一种水性高弹丙烯酸防水涂料及其制备方法。该水性高弹丙烯酸防水涂料包含以下重量份的成分:预制浆料30~45份,聚丙烯酸酯乳液40~55份,消泡剂0.1~0.3份,环保增塑剂3.0~7.0份,抗划痕剂0.6~1.0份,流变助剂0.6~1.0份。其制备方法包括:制备羧乙基醋酸丙酸纤维素、制备聚丙烯酸酯乳液、制备预制浆料和制备高弹丙烯酸防水涂料。该涂料颜色洁白,耐候性、耐黄变性佳,在人工曝晒老化加速2000h后,肉眼未发现颜色黄变,涂层未出现粉化、开裂、脱落现象。
Description
技术领域
本发明涉及建筑防水材料领域,具体为一种水性高弹丙烯酸防水涂料及其制备方法。
背景技术
防水涂料广泛用于建筑、道路桥梁设施、污水池、地下工程等领域。传统上,人们使用沥青油毡作为防水材料。由于沥青体系耐候性能有限,沥青油毡上方,需覆盖水泥砂浆或防护涂层。水泥砂浆较硬,长期日晒雨淋,温度变化易使砂浆层开裂、粉化,进而使防水层失效。合成树脂为主体的防护涂层具有良好的耐候性,是更好的技术方案。
目前,丙烯酸、聚氨酯等体系也被用作防水涂料的成膜物质。各体系各有特点。近年来,国家对环境保护空前重视,涂料领域水性化发展趋势日趋明显。防水涂料水性化也提上日程。具体到丙烯酸体系,该体系水汽屏蔽性能不如沥青,一般会与沥青体系复配使用。例如:中国专利申请CN 112646493A《一种高弹高粘的水乳型丙烯酸沥青防水涂料及其制备方法》,该专利申请即同时使用沥青与水性丙烯酸乳液。但由于沥青体系的特性,该方案涂料颜色一般为黑色,且颜色调整范围有限。又如:专利申请CN112961553A《一种单组份丙烯酸酯防水涂料及其制备方法》,该专利申请生产的防水涂料不含沥青体系,但该申请在树脂合成及消泡剂合成中均引入较大量的四氟乙烯,制备方法相对繁复。
因此,一款颜色自由可调,具有良好耐候性、持久高低温适应性、具有较强耐水性能,且生产工艺简便的水性丙烯酸防水涂料,具有宽广的的市场前景。
发明内容
本发明目的在于提供一种水性高弹丙烯酸防水涂料及其制备方法,该涂料颜色洁白,耐候性、耐黄变性佳,在人工曝晒老化加速2000h后,肉眼未发现颜色黄变,涂层未出现粉化、开裂、脱落现象。
本发明的技术方案是:
一种水性高弹丙烯酸防水涂料,包含以下重量份的成分:
所述的水性高弹丙烯酸防水涂料,包含以下重量份的成分:
所述的水性高弹丙烯酸防水涂料,消泡剂为矿物油、有机硅消泡剂中的一种或两种以上,环保增塑剂为柠檬酸三丁酯、乙酰柠檬酸三丁酯中的一种,抗划痕剂为高分子量的聚二甲基硅氧烷,流变助剂为聚氨酯类流变助剂、卡波姆类流变助剂中的一种或两种以上。
所述的水性高弹丙烯酸防水涂料,预制浆料包含以下重量份的成分:
所述的水性高弹丙烯酸防水涂料,分散剂为聚丙烯酸钠盐,润湿剂为聚醚硅氧烷共聚物,消泡剂为矿物油、有机硅消泡剂中的一种或两种以上,填料为硅微粉、石英粉、滑石粉中的一种或两种以上。
所述的水性高弹丙烯酸防水涂料,聚丙烯酸酯乳液包含以下重量份的成分:
所述的水性高弹丙烯酸防水涂料,乳化剂为十二烷基硫酸钠、十二烷基磺酸钠、十二烷基羧酸钠、硬脂酸钠、OP-10、OP-15、Tween-20和Tween-60中的一种或两种以上;引发剂为过硫酸钾、过硫酸铵中的一种;pH缓冲剂为碳酸氢钠。
所述的水性高弹丙烯酸防水涂料的制备方法,包含以下步骤:
(1)制备羧乙基醋酸丙酸纤维素
对羧乙基纤维素进行活化,得到具有反应活性的羧乙基纤维素;活化后的羧乙基纤维素在有机酸溶剂体系中,加入酯化液,经过酯化、水解、中和,水洗1~3次,得到羧乙基纤维素醋酸丙酸酯(CECAP);
(2)制备聚丙烯酸酯乳液
往预乳化釜依次加入1/4~1/2的去离子水、1/4~1/2的乳化剂、1/4~1/2的引发剂,搅拌至完全溶解,开启搅拌机,并控制预乳化釜温度为40~60℃、搅拌转速100~300rpm;往预乳化釜中依次加入甲基丙烯酸甲酯、甲基丙烯酸叔丁酯、甲基丙烯酸异冰片酯、丙烯酸正丁酯、丙烯酸异辛酯,搅拌转速100~300rpm,搅拌10~20min得到单体预乳化液;在装有搅拌、回流冷凝管的聚合釜内,依次加入剩余量的乳化剂、pH缓冲剂和剩余量的去离子水,开启搅拌机使之溶解,置于40~60℃水浴中;使用蠕动加料泵,把单体预乳化液滴加入聚合釜中,温度以0.5~2℃/min的速率升温至80~90℃;滴加完成后,补加剩余量的引发剂,继续保温1~3h后降至室温,过滤出料备用;
(3)制备预制浆料
往分散釜内加入乙二醇丁醚,开启搅拌机,调节搅拌转速至100~200rpm;加入羧乙基醋酸丙酸纤维素,调节搅拌机转速至250~350rpm,分散30~90min,直到完全溶解为止;加入二甲基乙醇胺中和,继续分散10~20min;加入1/4~1/2的去离子水,继续分散20~40min;过滤后,得到羧乙基醋酸丙酸纤维素预分散浆,备用;
往另一分散釜内加入剩余量的去离子水,开启搅拌机,搅拌转速100~300rpm,依次加入分散剂、润湿剂、消泡剂及上述羧乙基醋酸丙酸纤维素预分散浆;搅拌均匀,提升搅拌转速至300~400rpm,依次加入金红石型钛白粉和填料;搅拌分散30~60min后,检查浆料细度;浆料细度≤50μm时,停止搅拌、过滤、出料备用;
(4)制备高弹丙烯酸防水涂料
取步骤(2)制备的聚丙烯酸酯乳液至分散釜,开启搅拌机,搅拌转速100~300rpm,加入步骤(3)制备的预制浆料,搅拌10~30min至均匀;依次加入消泡剂、环保增塑剂、抗划痕剂、流变助剂,至搅拌均匀;100目滤网过滤、出料,得到高弹丙烯酸防水涂料。
所述的水性高弹丙烯酸防水涂料的制备方法,步骤(1)制备羧乙基醋酸丙酸纤维素时:
a、活化
将羧乙基纤维素浸没在醋酸中1~3次,然后浸没在丙酸中1~3次,每次10~30分钟,温度为30~50℃,然后密闭放置4~8h,得到具备反应活性的羧乙基纤维素;
b、酯化
按重量份数计,将100份活化后的羧乙基纤维素浸没在有机酸溶剂体系中,在5~15℃下加入250~350份酯化液,保温20~40min后,升温至30~50℃,保温50~100min,再升温至50~70℃,保温100~150min;加入15~25份浓度为15%~20wt%的醋酸,于50~100℃保温60~120min;
c、中和
按重量份数计,加入10~15份浓度为30~40%的醋酸镁水溶液或醋酸镁醋酸溶液,进行中和使pH值为5.5~6。
所述的水性高弹丙烯酸防水涂料的制备方法,有机酸溶剂为醋酸、丁酸中的一种或两种以上,酯化液为醋酸、丁酸、醋酸酐、丁酸酐、丙酸酐、浓硫酸中的一种或两种以上。
本发明的设计思想是:
本发明通过对羧乙基纤维素改性,得到羧乙基醋酸丙酸纤维素(CECAP),CECAP可有效减缓水性涂层体系中塑化剂向涂层表面迁移的过程,使涂层在自然环境下,能长时间保持良好的低温柔性性能,进而延长涂层防水性能失效时间。
本发明具有以下优点及有益效果:
1、本发明树脂合成过程中,不引入碳碳双键、苯环等不饱和结构,该涂料在户外使用,具有良好的耐候性和耐黄变性。
2、本发明引入环保塑化剂和抗划痕助剂,可使产品涂层在低温(-30~-20℃)下仍保持一定的柔韧性,同时在太阳直射高温下,涂层表面保持干爽不发粘,解决传统丙烯酸产品热黏冷脆的问题。
3、本发明引入羧乙基醋酸丙酸纤维素(CECAP),CECAP既可以加速涂层干燥过程,增强涂层抗紫外老化性能,又可提供适当的触变性能,增强罐内储存稳定性,还可以减缓上述环保塑化剂迁移速度,延缓产品涂层因塑化剂迁移而发脆失效,延长涂层寿命。
4、本发明不含沥青体系,颜色可根据实际需求自由调整。通过添加羧乙基醋酸丙酸纤维素,可以使漆膜长时间保持低温柔度。本发明所用原材料及丙烯酸树脂合成的原材料常温常压下均呈液态,生产工艺相对简单。所得涂料具有良好得不透水性,能在0.4MPa下耐水≥180min不渗水;优秀的柔韧性,-30℃下也能保持一定得柔韧性,且经过加速老化测试后,低温柔韧性仍能得到保持。
具体实施方式
在具体实施过程中,本发明提出的一种水性高弹丙烯酸防水涂料,包含以下重量份的成分:
优选的,所述预制浆料由以下原料组成:
优选的,所述聚丙烯酸酯乳液由以下原料组成:
上述技术方案通过控制丙烯酸软、硬单体比例、乳化剂种类及用量,控制合成工艺参数,所得聚丙烯酸酯乳液可在常温下成膜,且漆膜柔软,弹性佳。通过添加羧乙基醋酸丙酸纤维素,可以延缓塑化剂迁移离开涂层体系的过程,使涂层在较长时间内保持良好的低温柔度性能。
在此需要说明的是,对于这些实施方式的说明用于帮助理解本发明,但并不构成对本发明的限定。此外,下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例
在实施例中,水性高弹丙烯酸防水涂料的制备方法,包括如下步骤:
(1)制备羧乙基醋酸丙酸纤维素。对羧乙基纤维素进行活化,得到具备反应活性的羧乙基纤维素。活化后的羧乙基纤维素在有机酸溶剂体系中,加入酯化液,经过酯化、水解、中和,水洗2次,即可得到羧乙基纤维素醋酸丙酸酯(CECAP)。其中,有机酸溶剂为醋酸,酯化液为醋酸酐、丙酸酐和浓硫酸的混合物。
a、活化
将100份市售羧乙基纤维素浸没在浓度为15wt%的醋酸中2次,然后浸没在浓度为15wt%的丙酸中2次(每次浸泡,酸液与羧乙基纤维素的重量比为5:1),每次20分钟,温度为40℃,然后密闭放置6h,得到具备反应活性的羧乙基纤维素;
b、酯化
将活化后的羧乙基纤维素浸没在醋酸中,在10℃下加入酯化液(酯化液含有5份醋酸酐、312份丙酸酐和浓度98wt%的1.8份浓硫酸),保温30min后,升温至40℃,保温60min,再升温至60℃,保温120min;配制18份浓度为15wt%的醋酸,加入上述体系中,于60℃保温90min;
c、中和
加入12份浓度为35wt%的醋酸镁水溶液,调节体系pH至5.5~6。
(2)制备聚丙烯酸酯乳液。往预乳化釜依次加入1/2的去离子水、1/3的乳化剂、1/3的引发剂,搅拌至完全溶解。开启搅拌机,并控制预乳化釜温度为50℃、搅拌转速200rpm。往预乳化釜中依次加入甲基丙烯酸甲酯、甲基丙烯酸叔丁酯、甲基丙烯酸异冰片酯、丙烯酸正丁酯、丙烯酸异辛酯,搅拌转速200rpm,搅拌15min得到单体预乳化液。在装有搅拌、回流冷凝管的聚合釜内,依次加入剩余量的乳化剂、pH缓冲剂和剩余量的去离子水,开启搅拌机使之溶解,置于50℃水浴中。使用蠕动加料泵,以0.5g/s的速率,把单体预乳化液缓慢滴加入聚合釜中,温度以1℃/min的速率升温至82℃。滴加完成后,补加剩余量的引发剂,继续保温。保温2h后,降至室温,过滤出料备用。
(3)制备预制浆料。往分散釜内加入乙二醇丁醚,开启搅拌机,调节搅拌转速至150rpm。缓慢加入羧乙基醋酸丙酸纤维素,注意容器内壁上无残留。调节搅拌机转速至300rpm,分散60min,直到完全溶解为止。加入配方量二甲基乙醇胺,继续分散15min。缓慢加入1/2的去离子水,继续分散30min。过滤后,得到羧乙基醋酸丙酸纤维素预分散浆,备用。
往另一分散釜内加入剩余量的去离子水,开启搅拌机,搅拌转速200rpm,依次加入分散剂、润湿剂、消泡剂及上述羧乙基醋酸丙酸纤维素预分散浆。搅拌均匀,提升搅拌转速至350rpm,依次加入金红石型钛白粉和填料。搅拌分散45min后,检查浆料细度。浆料细度≤50μm时,停止搅拌、过滤、出料备用。
(14)制备高弹丙烯酸防水涂料。取上述聚丙烯酸酯乳液至分散釜,开启搅拌机,搅拌转速200rpm,加入上述预制浆料,搅拌20min至均匀。依次加入消泡剂、环保增塑剂、抗划痕剂、流变助剂,至搅拌均匀。100目滤网过滤、出料,即可得到高弹丙烯酸防水涂料。
各实施例重量份的成分如下表1所示:
表1各实施例及对比例重量份的成分
为展示实施例的性能,在实施例3基础上,不添加羧乙基醋酸丙酸纤维素,制备了对比例1,而后在对比例1基础上,进一步不添加乙酰柠檬酸三丁酯,制得对比例2。根据JC/T864-2008《聚合物乳液建筑防水涂料》,5.4.2节,分别把实施例1~3、对比例1~2制成涂膜。根据上述标准5.4.4节测试各样品标准条件下-10℃低温柔性性能,并参照上述5.4.3.3节人工气候老化处理方式,分别测试人工气候老化处理条件后,涂膜-10℃、-25℃低温柔度性能。测试结果如下表2所示:
表2各实施例及对比例低温柔度性能
测试结果显示,各实施例及对比例1,标准条件下-10℃低温柔度均无裂纹、无断裂,符合项目测试要求。对比例2因缺少乙酰柠檬酸三丁酯环保塑化剂,低温下丙烯酸酯聚合物发硬发脆的特性较明显,-10℃出现裂纹。比较实施例3与对比例1在人工气候老化处理条件下的低温柔度,缺少羧乙基醋酸丙酸纤维素的对比例1,经过照射168h紫外线后,低温柔度性能下降,原因可能是部分塑化剂在人工气候老化处理过程中,逐渐迁移至涂层表面,涂膜内部缺少塑化剂,致涂膜变脆。实施例中的羧乙基醋酸丙酸纤维素则能阻滞这一迁移过程,进而使实施例涂膜在人工气候老化处理后仍能保持良好的低温柔度。
Claims (10)
3.根据权利要求1至2之一所述的水性高弹丙烯酸防水涂料,其特征在于,消泡剂为矿物油、有机硅消泡剂中的一种或两种以上,环保增塑剂为柠檬酸三丁酯、乙酰柠檬酸三丁酯中的一种,抗划痕剂为高分子量的聚二甲基硅氧烷,流变助剂为聚氨酯类流变助剂、卡波姆类流变助剂中的一种或两种以上。
5.根据权利要求4所述的水性高弹丙烯酸防水涂料,其特征在于,分散剂为聚丙烯酸钠盐,润湿剂为聚醚硅氧烷共聚物,消泡剂为矿物油、有机硅消泡剂中的一种或两种以上,填料为硅微粉、石英粉、滑石粉中的一种或两种以上。
7.根据权利要求6所述的水性高弹丙烯酸防水涂料,其特征在于,乳化剂为十二烷基硫酸钠、十二烷基磺酸钠、十二烷基羧酸钠、硬脂酸钠、OP-10、OP-15、Tween-20和Tween-60中的一种或两种以上;引发剂为过硫酸钾、过硫酸铵中的一种;pH缓冲剂为碳酸氢钠。
8.一种权利要求1~7之一所述的水性高弹丙烯酸防水涂料的制备方法,其特征在于,包含以下步骤:
(1)制备羧乙基醋酸丙酸纤维素
对羧乙基纤维素进行活化,得到具有反应活性的羧乙基纤维素;活化后的羧乙基纤维素在有机酸溶剂体系中,加入酯化液,经过酯化、水解、中和,水洗1~3次,得到羧乙基纤维素醋酸丙酸酯(CECAP);
(2)制备聚丙烯酸酯乳液
往预乳化釜依次加入1/4~1/2的去离子水、1/4~1/2的乳化剂、1/4~1/2的引发剂,搅拌至完全溶解,开启搅拌机,并控制预乳化釜温度为40~60℃、搅拌转速100~300rpm;往预乳化釜中依次加入甲基丙烯酸甲酯、甲基丙烯酸叔丁酯、甲基丙烯酸异冰片酯、丙烯酸正丁酯、丙烯酸异辛酯,搅拌转速100~300rpm,搅拌10~20min得到单体预乳化液;在装有搅拌、回流冷凝管的聚合釜内,依次加入剩余量的乳化剂、pH缓冲剂和剩余量的去离子水,开启搅拌机使之溶解,置于40~60℃水浴中;使用蠕动加料泵,把单体预乳化液滴加入聚合釜中,温度以0.5~2℃/min的速率升温至80~90℃;滴加完成后,补加剩余量的引发剂,继续保温1~3h后降至室温,过滤出料备用;
(3)制备预制浆料
往分散釜内加入乙二醇丁醚,开启搅拌机,调节搅拌转速至100~200rpm;加入羧乙基醋酸丙酸纤维素,调节搅拌机转速至250~350rpm,分散30~90min,直到完全溶解为止;加入二甲基乙醇胺中和,继续分散10~20min;加入1/4~1/2的去离子水,继续分散20~40min;过滤后,得到羧乙基醋酸丙酸纤维素预分散浆,备用;
往另一分散釜内加入剩余量的去离子水,开启搅拌机,搅拌转速100~300rpm,依次加入分散剂、润湿剂、消泡剂及上述羧乙基醋酸丙酸纤维素预分散浆;搅拌均匀,提升搅拌转速至300~400rpm,依次加入金红石型钛白粉和填料;搅拌分散30~60min后,检查浆料细度;浆料细度≤50μm时,停止搅拌、过滤、出料备用;
(4)制备高弹丙烯酸防水涂料
取步骤(2)制备的聚丙烯酸酯乳液至分散釜,开启搅拌机,搅拌转速100~300rpm,加入步骤(3)制备的预制浆料,搅拌10~30min至均匀;依次加入消泡剂、环保增塑剂、抗划痕剂、流变助剂,至搅拌均匀;100目滤网过滤、出料,得到高弹丙烯酸防水涂料。
9.根据权利要求8所述的水性高弹丙烯酸防水涂料的制备方法,其特征在于,步骤(1)制备羧乙基醋酸丙酸纤维素时:
a、活化
将羧乙基纤维素浸没在醋酸中1~3次,然后浸没在丙酸中1~3次,每次10~30分钟,温度为30~50℃,然后密闭放置4~8h,得到具备反应活性的羧乙基纤维素;
b、酯化
按重量份数计,将100份活化后的羧乙基纤维素浸没在有机酸溶剂体系中,在5~15℃下加入250~350份酯化液,保温20~40min后,升温至30~50℃,保温50~100min,再升温至50~70℃,保温100~150min;加入15~25份浓度为15%~20wt%的醋酸,于50~100℃保温60~120min;
c、中和
按重量份数计,加入10~15份浓度为30~40%的醋酸镁水溶液或醋酸镁醋酸溶液,进行中和使pH值为5.5~6。
10.根据权利要求9所述的水性高弹丙烯酸防水涂料的制备方法,其特征在于,有机酸溶剂为醋酸、丁酸中的一种或两种以上,酯化液为醋酸、丁酸、醋酸酐、丁酸酐、丙酸酐、浓硫酸中的一种或两种以上。
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