CN114524903A - 一种低温恶劣环境下弹性涂料用水性树脂及其制备方法 - Google Patents
一种低温恶劣环境下弹性涂料用水性树脂及其制备方法 Download PDFInfo
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- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
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- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 2
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种低温恶劣环境下弹性涂料用水性树脂及其制备方法,先向聚合釜中加入一部分软水、乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;然后向聚合釜中加入一部分软水、pH值调节剂、乳化单体、乳化剂,加入引发剂,加热反应,再匀速缓慢滴加剩余配方原料,加热搅拌反应,降温,消除残余单体,加入消泡剂,搅拌混匀,降温,调节pH,过滤,即得水性树脂。本发明所得水性树脂具有较低的玻璃化温度,即使在低温条件下也能保持一定的延伸率起到遮盖裂缝的效果,可用于低温恶劣环境下弹性涂料的制备。
Description
技术领域
本发明涉及一种,具体涉及一种低温恶劣环境下弹性涂料用水性树脂及其制备方法。属于技术领域。
背景技术
弹性涂料除了具有一般保护和装饰功能外,同时具有较强的遮盖裂缝能力。如果选用性能优良的改性弹性乳液则可明显提高弹性涂料的耐沾污性和抗水性,因此弹性涂料越来越受到用户的喜爱和市场青睐。弹性涂料的组成配方和生产与乳胶漆基本相似,均采用优质丙烯酸乳液为成膜物质,配套各种颜填料和功能助剂而成。但其独特之处在于所用乳液不同,弹性涂料所选用的丙烯酸乳液其特点首先在于具有较低的玻璃化温度(Tg=-22℃),即使在低温条件下也能保持一定的延伸率起到遮盖裂缝的效果,同时采用特殊的交联单体以提高耐沾污性和抗水性。
发明内容
本发明的目的是为克服上述现有技术的不足,提供一种低温恶劣环境下弹性涂料用水性树脂及其制备方法。
为实现上述目的,本发明采用下述技术方案:
一种低温恶劣环境下弹性涂料用水性树脂的制备方法,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、60~70%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、10~30%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料,81~83℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.1~0.2%的消泡剂,搅拌混匀,降温至40℃,调节pH=7~9,过滤,即得所述的水性树脂;
以重量份计,配方原料组成如下:混合单体100份,乳化剂0.7~4份,pH值调节剂1~2份,引发剂0.1~1份,链转移剂0.1~1份,软水80~100份。
优选的,步骤(2)中,剩余配方原料的滴加时间为3小时。
优选的,以重量份计,所述混合单体是由以下组分混合而成:丙烯酸酯单体80~90份,不饱和羧酸1.5~3份,不饱和酰胺2~5份,1-十八(碳)烯0.5~2份。
进一步优选的,所述丙烯酸酯化合物选自丙烯酸丁酯、丙烯酸辛酯或甲基丙烯酸甲酯中的任一种或多种,所述不饱和羧酸选自丙烯酸、甲基丙烯酸、衣康酸或马来酸酐中的任一种或多种,所述不饱和酰胺选自丙烯酰胺、甲基丙烯酰胺、二甲基丙烯酰胺、羟甲基丙烯酰胺或甲基羟甲基丙烯酰胺中的任一种或多种。
优选的,以重量份计,所述复合乳化剂是将以下组分混合而成:阴离子乳化剂0.5~2份,非离子乳化剂0.2~2份。
进一步优选的,所述阴离子乳化剂为烷基硫酸盐或烷基磺酸盐,所述非离子乳化剂为烷基酚聚氧乙烯醚或脂肪醇聚氧乙烯醚。
优选的,所述pH值调节剂为质量浓度10~12%氨水溶液,所述引发剂为过硫酸钾或过硫酸铵,所述催化剂为亚硫酸氢钠或焦亚硫酸钠,所述消泡剂为有机硅消泡剂,所述链转移剂为脂肪族硫醇或十二烷基硫醇。
优选的,步骤(2)中,在加入剩余配方原料时还加入添加剂,其加入量为混合单体总质量的1~2%;以重量份计,添加剂的制备方法如下:
(A)先将0.5~0.7份氯化铝、0.5~0.7份醋酸锡超声波分散于10份水中,得到水分散液,接着向水分散液中加入0.05~0.07硫化钠、0.04~0.05份质量浓度25~28%浓氨水,超声波分散均匀,得到预混液;再将预混液经水热反应,后处理,得到多孔纳米材料;
(B)再将多孔纳米材料利用γ-甲基丙烯酰氧基丙基三甲氧基硅烷进行改性处理,得到添加剂。
进一步优选的,步骤(A)中,水热反应的工艺条件为:150~160℃水热反应7~8小时;后处理包括:离心,洗涤,冷冻干燥。
进一步优选的,以重量份计,步骤(B)的具体方法如下:先将5~7份多孔纳米材料加入20~22份γ-甲基丙烯酰氧基丙基三甲氧基硅烷中,85~95℃搅拌反应5~6小时,离心取沉淀,即得添加剂。
利用上述制备方法得到的一种低温恶劣环境下弹性涂料用水性树脂。
本发明的有益效果:
本发明先向聚合釜中加入一部分软水、乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;然后向聚合釜中加入一部分软水、pH值调节剂、乳化单体、乳化剂,加入引发剂,加热反应,再匀速缓慢滴加剩余配方原料,加热搅拌反应,降温,消除残余单体,加入消泡剂,搅拌混匀,降温,调节pH,过滤,即得水性树脂。本发明所得水性树脂具有较低的玻璃化温度,即使在低温条件下也能保持一定的延伸率起到遮盖裂缝的效果,可用于低温恶劣环境下弹性涂料的制备。
本发明还加入添加剂,该添加剂的制备方法如下:先将碳纳米管超声波分散于水中,得到水分散液,接着向水分散液中加入硫化钠、浓氨水、氯化铝、醋酸锡,超声波分散均匀,得到预混液;再将预混液经水热反应,后处理,得到多孔纳米材料;再将多孔纳米材料利用γ-甲基丙烯酰氧基丙基三甲氧基硅烷进行改性处理,即得。多孔纳米材料实质上是铝、锡氧化物部分缺陷化并与碳纳米管的复合物,比表面积大,通过γ-甲基丙烯酰氧基丙基三甲氧基硅烷改性处理后引入双键,可参与聚合反应,在体系中的相容性好,进一步改善产品性能。
具体实施方式
下面结合实施例对本发明进行进一步的阐述,应该说明的是,下述说明仅是为了解释本发明,并不对其内容进行限定。
实施例1:
一种低温恶劣环境下弹性涂料用水性树脂的制备方法,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、60%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、10%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料,81℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.1%的消泡剂,搅拌混匀,降温至40℃,调节pH=7,过滤,即得所述的水性树脂;
配方原料组成如下:混合单体100g,乳化剂0.7g,pH值调节剂1g,引发剂0.1g,链转移剂0.1g,软水80g。
步骤(2)中,剩余配方原料的滴加时间为3小时。
所述混合单体是由以下组分混合而成:丙烯酸酯单体80g,不饱和羧酸1.5g,不饱和酰胺2g,1-十八(碳)烯0.5g。
所述丙烯酸酯化合物为丙烯酸丁酯,所述不饱和羧酸为丙烯酸,所述不饱和酰胺为丙烯酰胺。
所述复合乳化剂是将以下组分混合而成:十二烷基硫酸钠0.5g,烷基聚氧乙烯醚(10)0.2g。
所述pH值调节剂为质量浓度10%氨水溶液,所述引发剂为过硫酸钾,所述消泡剂为有机硅消泡剂。
实施例2:
一种低温恶劣环境下弹性涂料用水性树脂的制备方法,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、70%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、30%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料, 83℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.2%的消泡剂,搅拌混匀,降温至40℃,调节pH=9,过滤,即得所述的水性树脂;
配方原料组成如下:混合单体100g,乳化剂4g,pH值调节剂2g,引发剂1g,链转移剂1g,软水100g。
步骤(2)中,剩余配方原料的滴加时间为3小时。
所述混合单体是由以下组分混合而成:丙烯酸酯单体90g,不饱和羧酸3g,不饱和酰胺5g,1-十八(碳)烯2g。
所述丙烯酸酯化合物为丙烯酸辛酯,所述不饱和羧酸为衣康酸,所述不饱和酰胺为甲基丙烯酰胺。
所述复合乳化剂是将以下组分混合而成:十二烷基苯磺酸钠2g,烷基聚氧乙烯醚(40)2g。
所述pH值调节剂为质量浓度12%氨水溶液,所述引发剂为过硫酸钾,所述消泡剂为有机硅消泡剂。
实施例3:
一种低温恶劣环境下弹性涂料用水性树脂的制备方法,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、65%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、20%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料,82℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.15%的消泡剂,搅拌混匀,降温至40℃,调节pH=8,过滤,即得所述的水性树脂;
配方原料组成如下:混合单体100g,乳化剂2g,pH值调节剂1.5g,引发剂0.8g,链转移剂0.5g,软水90g。
步骤(2)中,剩余配方原料的滴加时间为3小时。
所述混合单体是由以下组分混合而成:丙烯酸丁酯80g,甲基丙烯酸甲酯5g,衣康酸1.5g,马来酸酐1g,羟甲基丙烯酰胺2g,甲基羟甲基丙烯酰胺2g,1-十八(碳)烯1.5g。
所述复合乳化剂是将以下组分混合而成:十二烷基硫酸钠1g,烷基二苯基氧化物二磺酸钠0.5g,烷基聚氧乙烯醚(30)1g,烷基聚氧乙烯醚(40)0.5g。
所述pH值调节剂为质量浓度11%氨水溶液,所述引发剂为过硫酸铵,所述消泡剂为有机硅消泡剂。
步骤(2)中,在加入剩余配方原料时还加入添加剂,其加入量为混合单体总质量的1%;添加剂的制备方法如下:
(A)先将0.5g氯化铝、0.5g醋酸锡超声波分散于10g水中,得到水分散液,接着向水分散液中加入0.05硫化钠、0.04g质量浓度25%浓氨水,超声波分散均匀,得到预混液;再将预混液经水热反应,后处理,得到多孔纳米材料;
(B)再将多孔纳米材料利用γ-甲基丙烯酰氧基丙基三甲氧基硅烷进行改性处理,得到添加剂。
步骤(A)中,水热反应的工艺条件为:150℃水热反应7小时;后处理包括:离心,洗涤,冷冻干燥。
步骤(B)的具体方法如下:先将5g多孔纳米材料加入20gγ-甲基丙烯酰氧基丙基三甲氧基硅烷中,85℃搅拌反应5小时,离心取沉淀,即得添加剂。
实施例4:
一种低温恶劣环境下弹性涂料用水性树脂的制备方法,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、65%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、20%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料,82℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.15%的消泡剂,搅拌混匀,降温至40℃,调节pH=8,过滤,即得所述的水性树脂;
配方原料组成如下:混合单体100g,乳化剂2g,pH值调节剂1.5g,引发剂0.8g,链转移剂0.5g,软水90g。
步骤(2)中,剩余配方原料的滴加时间为3小时。
所述混合单体是由以下组分混合而成:丙烯酸丁酯70g,丙烯酸辛酯10g,甲基丙烯酸甲酯5g,丙烯酸1g,甲基丙烯酸1g,衣康酸0.2g,马来酸酐0.3g,丙烯酰1g,甲基丙烯酰胺1g,二甲基丙烯酰胺1g,羟甲基丙烯酰胺1g,1-十八(碳)烯1.5g。
所述复合乳化剂是将以下组分混合而成:十二烷基硫酸钠0.1g,十二烷基苯磺酸钠0.1g,烷基二苯基氧化物二磺酸钠0.1g,烷基聚氧乙烯醚(10)0.2g,烷基聚氧乙烯醚(30)0.5g,烷基聚氧乙烯醚(40)0.5g。
所述pH值调节剂为质量浓度11%氨水溶液,所述引发剂为过硫酸钾,所述消泡剂为有机硅消泡剂。
步骤(2)中,在加入剩余配方原料时还加入添加剂,其加入量为混合单体总质量的2%;添加剂的制备方法如下:
(A)先将0.7g氯化铝、0.7g醋酸锡超声波分散于10g水中,得到水分散液,接着向水分散液中加入0.07硫化钠、0.05g质量浓度28%浓氨水,超声波分散均匀,得到预混液;再将预混液经水热反应,后处理,得到多孔纳米材料;
(B)再将多孔纳米材料利用γ-甲基丙烯酰氧基丙基三甲氧基硅烷进行改性处理,得到添加剂。
步骤(A)中,水热反应的工艺条件为: 160℃水热反应8小时;后处理包括:离心,洗涤,冷冻干燥。
步骤(B)的具体方法如下:先将7g多孔纳米材料加入22gγ-甲基丙烯酰氧基丙基三甲氧基硅烷中, 95℃搅拌反应6小时,离心取沉淀,即得添加剂。
试验例
对实施例1~4所得水性树脂进行基本性能检测。
其中,固含量参考GB/T 1725-2007进行检测,粘度使用粘度计进行检测,玻璃化温度使用玻璃化转变温度测试仪(DSC法)确定;并参考GB/T 16777-2008考察水性树脂的防水性,结果见表1。
表1. 性能测试结果
固含量(%) | 粘度(mPa·s) | 玻璃化转变温度(℃) | -10℃低温柔性 | 0.3MPa,0.5h,不透水性 | |
实施例1 | 50.7 | 95 | -20 | 无裂痕 | 不透水 |
实施例2 | 50.6 | 96 | -21 | 无裂痕 | 不透水 |
实施例3 | 50.9 | 111 | -27 | 无裂痕 | 不透水 |
实施例4 | 51.1 | 117 | -30 | 无裂痕 | 不透水 |
由表1可知,实施例1~4所得水性树脂的固含量高,粘度高,玻璃化温度低,-10℃低温柔性佳,且具有较好的耐水性,可适应低温恶劣环境下弹性涂料用。特别是实施例3、4加入了添加剂,各项性能更佳。
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (9)
1.一种低温恶劣环境下弹性涂料用水性树脂的制备方法,其特征在于,以质量百分比计,具体步骤如下:
(1)先向聚合釜中加入30%配方量的软水、60~70%配方量的乳化剂,接着边搅拌边加入混合单体,搅拌乳化均匀,得到乳化单体;
(2)然后向聚合釜中加入50%配方量的软水、50%配方量的pH值调节剂、步骤(1)所得乳化单体质量的5%、10~30%配方量的乳化剂,升温至80℃,加入20%配方量的引发剂,保温搅拌反应15分钟,再匀速缓慢滴加剩余配方原料,81~83℃搅拌反应1小时,降温至75℃,消除残余单体,加入混合单体总质量0.1~0.2%的消泡剂,搅拌混匀,降温至40℃,调节pH=7~9,过滤,即得所述的水性树脂;
以重量份计,配方原料组成如下:混合单体100份,乳化剂0.7~4份,pH值调节剂1~2份,引发剂0.1~1份,链转移剂0.1~1份,软水80~100份。
2.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,剩余配方原料的滴加时间为3小时。
3.根据权利要求1所述的制备方法,其特征在于,以重量份计,所述混合单体是由以下组分混合而成:丙烯酸酯单体80~90份,不饱和羧酸1.5~3份,不饱和酰胺2~5份,1-十八(碳)烯0.5~2份。
4.根据权利要求3所述的制备方法,其特征在于,所述丙烯酸酯化合物选自丙烯酸丁酯、丙烯酸辛酯或甲基丙烯酸甲酯中的任一种或多种,所述不饱和羧酸选自丙烯酸、甲基丙烯酸、衣康酸或马来酸酐中的任一种或多种,所述不饱和酰胺选自丙烯酰胺、甲基丙烯酰胺、二甲基丙烯酰胺、羟甲基丙烯酰胺或甲基羟甲基丙烯酰胺中的任一种或多种。
5.根据权利要求1所述的制备方法,其特征在于,以重量份计,所述复合乳化剂是将以下组分混合而成:阴离子乳化剂0.5~2份,非离子乳化剂0.2~2份。
6.根据权利要求5所述的制备方法,其特征在于,所述阴离子乳化剂为烷基硫酸盐或烷基磺酸盐,所述非离子乳化剂为烷基酚聚氧乙烯醚或脂肪醇聚氧乙烯醚。
7.根据权利要求1所述的制备方法,其特征在于,所述pH值调节剂为质量浓度10~12%氨水溶液,所述引发剂为过硫酸钾或过硫酸铵,所述催化剂为亚硫酸氢钠或焦亚硫酸钠,所述消泡剂为有机硅消泡剂,所述链转移剂为脂肪族硫醇或十二烷基硫醇。
8.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,在加入剩余配方原料时还加入添加剂,其加入量为混合单体总质量的1~2%;以重量份计,添加剂的制备方法如下:
(A)先将0.5~0.7份氯化铝、0.5~0.7份醋酸锡超声波分散于10份水中,得到水分散液,接着向水分散液中加入0.05~0.07硫化钠、0.04~0.05份质量浓度25~28%浓氨水,超声波分散均匀,得到预混液;再将预混液经水热反应,后处理,得到多孔纳米材料;
(B)再将多孔纳米材料利用γ-甲基丙烯酰氧基丙基三甲氧基硅烷进行改性处理,得到添加剂。
9.利用权利要求1~8中任一项所述制备方法得到的一种低温恶劣环境下弹性涂料用水性树脂。
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