CN113736423A - 一种建筑用高耐候性密封胶的制备方法 - Google Patents
一种建筑用高耐候性密封胶的制备方法 Download PDFInfo
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- CN113736423A CN113736423A CN202111075074.8A CN202111075074A CN113736423A CN 113736423 A CN113736423 A CN 113736423A CN 202111075074 A CN202111075074 A CN 202111075074A CN 113736423 A CN113736423 A CN 113736423A
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Abstract
本发明涉及一种建筑用高耐候性密封胶的制备方法,属于密封胶制备技术领域,包括以下步骤:第一步、准备各组重量份原料;第二步、将低聚物多元醇、异氰酸酯单体、亲水改性剂、功能填料、催化剂和有机溶剂按照配方量加入反应釜中,升温至50‑90℃,搅拌反应40‑60min,得到第一混料;第三步、将第一混料降温至20‑40℃,加入扩链剂和去离子水混合后,加入pH调节剂和增稠剂,搅拌1.5‑2.5h,得到建筑用高耐候性密封胶,本发明的密封胶以水为溶剂,环保健康,通过加入自制的功能粒子提高密封胶的保温、隔音、防水、耐候性能,在建筑材料中具有很大的应用价值。
Description
技术领域
本发明属于密封胶制备技术领域,具体地,涉及一种建筑用高耐候性密封胶的制备方法。
背景技术
建筑外墙填缝密封胶直接影响建筑外墙的水密性、气密性、隔声性和抗风压性,对建筑外墙密封起重要影响,是土木建筑外墙系统的重要组成部分。
聚氨酯密封胶和硅酮密封胶是目前普遍使用的外墙填缝密封胶,虽然硅酮密封胶的耐候性好,具有较高的使用性能,但其在应用过程中有一定概率出现建筑外墙板开裂或漏水等问题,且硅酮密封胶使用过程中硅油外渗污染建筑物,维修过程中外渗的硅油发挥脱模剂功能,在一定程度上造成硅酮密封胶与建筑基材粘接的可靠性下降,对使用造成影响,聚氨酯密封胶分子链中存在C-H、C-N、C-O等弱化学键,它们对光、热、氧比较敏感,在存储和使用过程中会发生老化,影响密封胶的综合性能,因此,提出一种耐候性好、综合性能高的建筑用密封胶是目前需要解决的技术问题。
发明内容
本发明的目的在于提供一种建筑用高耐候性密封胶的制备方法,以解决背景技术中所提出的技术问题。
本发明的目的可以通过以下技术方案实现:
一种建筑用高耐候性密封胶的制备方法,包括以下步骤:
第一步、准备以下重量份原料:低聚物多元醇15-20份、异氰酸酯单体5-13份、亲水改性剂0.8-1.5份、功能填料3.7-5.8份、pH调节剂0.1-0.5份、扩链剂0.5-3.0份、催化剂0.01-0.04份、有机溶剂3-11份、去离子水50-80份、增稠剂0.5-2份;
第二步、将低聚物多元醇、异氰酸酯单体、亲水改性剂、功能填料、催化剂和有机溶剂按照配方量加入反应釜中,升温至50-90℃,搅拌反应40-60min,得到第一混料;
第三步、将第一混料降温至20-40℃,加入扩链剂和去离子水,转速200-300r/min条件下,混合1h,最后加入pH调节剂和增稠剂,搅拌1.5-2.5h,得到建筑用高耐候性密封胶。
进一步地,低聚物多元醇为聚己二酸丁二醇酯二元醇、聚碳酸酯二元醇、聚己内酯二元醇、聚四氢呋喃醚二醇和聚四亚甲基醚二醇中的一种或多种按任意比例混合而成,数均分子量为1000-3000。
进一步地,亲水改性剂为二羟甲基丙烯和二羟甲基丁酸中的一种。
进一步地,异氰酸酯单体为HDI、MDI、IPDI和HMDI中的一种或多种按任意比例混合而成。
进一步地,催化剂为月桂酸二丁基锡、醋酸锂、三正丁基锂和二乙酸二丁基锡中的一种或多种按任意比例混合而成。
进一步地,增稠剂为缔合型疏水改性的聚氨酯增稠剂。
进一步地,有机溶剂为N-甲基吡咯烷酮、丙酮和丁酮中的一种或多种按任意比例混合而成。
进一步地,扩链剂为乙二醇、1,2-丙二醇、1,4-丁二醇、新戊二醇和二甘醇中的一种或多种按任意比例混合而成。
进一步地,pH调节剂为三乙胺、醋酸和赖氨酸中的一种。
进一步地,功能填料由以下步骤制成:
步骤1、氮气保护下,将环氧氯丙烷、3,5-二叔丁基-4-羟基苯甲醇和二甲基亚砜加入三口烧瓶中,控制温度50-60℃,搅拌反应10min,然后加入氢氧化钾,回流反应3-5h,反应结束后,制得中间产物1,然后控制反应温度0-5℃,向三口烧瓶中滴加4-氨基-1,2,2,6,6-五甲基哌啶,1h内滴加结束,滴加结束后升温至19-21℃,搅拌反应2h,反应结束后,过滤,滤液用去离子水洗涤,之后乙酸乙酯萃取,旋蒸去除乙酸乙酯,制得中间产物2;
其中环氧氯丙烷、3,5-二叔丁基-4-羟基苯甲醇、二甲基亚砜、4-氨基-1,2,2,6,6-五甲基哌啶的用量比为50mmol:50mmol:48.6-52.3mL:50mmol,氢氧化钾的用量为3,5-二叔丁基-4-羟基苯甲醇质量的4-6%;
在碱性条件下,使环氧氯丙烷和3,5-二叔丁基-4-羟基苯甲醇发生开环反应得到中间产物1,然后使中间产物1与4-氨基-1,2,2,6,6-五甲基哌啶发生消去HC l的反应得到中间产物2,反应过程如下:
步骤2、将中间产物2和丙烯酸加入反应釜中,进行搅拌并加入浓硫酸,在温度为80-90℃的条件下,进行反应2-3h,反应结束后,加入去离子水洗涤,用乙酸乙酯萃取后,旋蒸去除乙酸乙酯,制得改性剂;
其中,中间产物2和丙烯酸的用量摩尔比为1:2-3,浓硫酸的用量为中间产物2和丙烯酸总质量的2-4%,浓硫酸质量分数为95%;
在浓硫酸的催化作用下,使中间产物2和丙烯酸发生酯化反应得到改性剂,反应过程如下:
步骤3、将中空玻璃微珠加入浓度0.3mol/L的氢氧化钠溶液中搅拌1.5h后,过滤,滤饼用蒸馏水洗涤至洗涤液呈中性,再于70℃烘箱中干燥至恒重,得到刻蚀玻璃微珠,其中中空玻璃微珠和氢氧化钠溶液的用量比为1g:30mL;
步骤4、将刻蚀玻璃微珠、水和乙醇加入圆底烧瓶中,频率40-50kHz下超声分散20-40min,然后加入硝酸锌的乙醇溶液,搅拌10min后,加入氢氧化钠,室温搅拌反应30-60min,反应结束后,抽滤,滤饼用去离子水洗涤至中性,于70℃下干燥12h后,再于400℃下煅烧30min后,冷却至室温,得到包覆玻璃微珠;其中刻蚀玻璃微珠、水、乙醇、硝酸锌的乙醇溶液和氢氧化钠的用量比为6.2-6.8g:20-30mL:15-20mL:3-5mL:0.3-0.6g,硝酸锌的乙醇溶液由硝酸锌和乙醇按照1g:5mL混合而成;
步骤5、将包覆玻璃微珠和乙醇加入圆底烧瓶中,超声分散20min后,加入偶联剂KH-590,搅拌反应2-4h后,加入甲基丙烯酸三氟乙酯、改性剂和安息香双甲醚,紫外灯照射下,搅拌反应30-60min,反应结束后,抽滤,滤饼用去离子水洗涤3-5次,最后于60℃烘箱中干燥至恒重,得到功能填料,其中包覆玻璃微珠、乙醇、偶联剂KH-590、甲基丙烯酸三氟乙酯、改性剂和安息香双甲醚的用量比为5.6-6.7g:60-80mL:1.2-1.5g:0.5-0.8g:0.2-0.4g:0.1-0.3g。
本发明的有益效果:
本发明以低聚物多元醇、异氰酸酯单体、功能填料和助剂为原料制备了一种聚氨酯密封胶,以水为溶剂,环保健康,通过加入功能填料提高密封胶的保温、隔音、防水、耐候性能,首先利用化学手段合成改性剂,然后使中空玻璃微珠在氢氧化钠溶液中刻蚀得到刻蚀玻璃微珠,再于刻蚀玻璃微珠表面包覆氧化锌层,通过偶联剂KH-590改性后,与甲基丙烯酸三氟乙酯、改性剂在紫外灯照射下发生接枝反应,得到功能填料,其中中空玻璃微珠具有表面积大、隔音、隔热等优点,氧化锌属于N型半导体,价带上的电子可以接受紫外线中的能量发生跃迁,对紫外线有吸收和散射作用,并且具有抗菌作用,改性剂中含有受阻酚和受阻胺结构,具有抗氧化作用,并且接枝于包覆玻璃微珠表面,不易迁移,甲基丙烯酸三氟乙酯含有F-C键,F-C键键长短,键能高,将功能粒子加入聚氨酯密封胶中,中空玻璃微珠使其具有隔音、隔热性能,氧化锌和改性剂赋予其较高的抗氧化性能,F-C键的存在,使聚氨酯表面的自由能较低,具有较高的防水、耐候性。
具体实施方式
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它实施例,都属于本发明保护的范围。
实施例1
本实施例制备一种功能填料,步骤如下:
步骤1、氮气保护下,将50mmol环氧氯丙烷、50mmol 3,5-二叔丁基-4-羟基苯甲醇和48.6mL二甲基亚砜加入三口烧瓶中,控制温度50℃,搅拌反应10min,然后加入氢氧化钾,回流反应3h,反应结束后,制得中间产物1,然后控制反应温度0℃,向三口烧瓶中滴加50mmol 4-氨基-1,2,2,6,6-五甲基哌啶,1h内滴加结束,滴加结束后升温至19℃,搅拌反应2h,反应结束后,过滤,滤液用去离子水洗涤,之后乙酸乙酯萃取,旋蒸去除乙酸乙酯,制得中间产物2,氢氧化钾的用量为3,5-二叔丁基-4-羟基苯甲醇质量的4%;
步骤2、将0.1mol中间产物2和0.2mol丙烯酸加入反应釜中,进行搅拌并加入浓硫酸,在温度为80℃的条件下,进行反应2h,反应结束后,加入去离子水洗涤,用乙酸乙酯萃取后,旋蒸去除乙酸乙酯,制得改性剂,浓硫酸的用量为中间产物2和丙烯酸总质量的2%;
步骤3、将中空玻璃微珠加入浓度0.3mol/L的氢氧化钠溶液中搅拌1.5h后,过滤,滤饼用蒸馏水洗涤至洗涤液呈中性,再于70℃烘箱中干燥至恒重,得到刻蚀玻璃微珠,其中中空玻璃微珠和氢氧化钠溶液的用量比为1g:30mL;
步骤4、将6.2g刻蚀玻璃微珠、20mL水和15mL乙醇加入圆底烧瓶中,频率40kHz下超声分散20min,然后加入3mL硝酸锌的乙醇溶液,搅拌10min后,加入0.3g氢氧化钠,室温搅拌反应30min,反应结束后,抽滤,滤饼用去离子水洗涤至中性,于70℃下干燥12h后,再于400℃下煅烧30min后,冷却至室温,得到包覆玻璃微珠;硝酸锌的乙醇溶液由硝酸锌和乙醇按照1g:5mL混合而成;
步骤5、将5.6g包覆玻璃微珠和60mL乙醇加入圆底烧瓶中,超声分散20min后,加入1.2g偶联剂KH-590,搅拌反应2h后,加入0.5g甲基丙烯酸三氟乙酯、0.2g改性剂和0.1g安息香双甲醚,紫外灯照射下,搅拌反应30min,反应结束后,抽滤,滤饼用去离子水洗涤3次,最后于60℃烘箱中干燥至恒重,得到功能填料。
实施例2
本实施例制备一种功能填料,步骤如下:
步骤1、氮气保护下,将50mmol环氧氯丙烷、50mmol 3,5-二叔丁基-4-羟基苯甲醇和49.1mL二甲基亚砜加入三口烧瓶中,控制温度55℃,搅拌反应10min,然后加入氢氧化钾,回流反应4h,反应结束后,制得中间产物1,然后控制反应温度3℃,向三口烧瓶中滴加50mmol 4-氨基-1,2,2,6,6-五甲基哌啶,1h内滴加结束,滴加结束后升温至20℃,搅拌反应2h,反应结束后,过滤,滤液用去离子水洗涤,之后乙酸乙酯萃取,旋蒸去除乙酸乙酯,制得中间产物2,氢氧化钾的用量为3,5-二叔丁基-4-羟基苯甲醇质量的5%;
步骤2、将0.1mol中间产物2和0.25mol丙烯酸加入反应釜中,进行搅拌并加入浓硫酸,在温度为85℃的条件下,进行反应2.5h,反应结束后,加入去离子水洗涤,用乙酸乙酯萃取后,旋蒸去除乙酸乙酯,制得改性剂,浓硫酸的用量为中间产物2和丙烯酸总质量的3%;
步骤3、将中空玻璃微珠加入浓度0.3mol/L的氢氧化钠溶液中搅拌1.5h后,过滤,滤饼用蒸馏水洗涤至洗涤液呈中性,再于70℃烘箱中干燥至恒重,得到刻蚀玻璃微珠,其中中空玻璃微珠和氢氧化钠溶液的用量比为1g:30mL;
步骤4、将6.4g刻蚀玻璃微珠、25mL水和18mL乙醇加入圆底烧瓶中,频率48kHz下超声分散30min,然后加入4mL硝酸锌的乙醇溶液,搅拌10min后,加入0.4g氢氧化钠,室温搅拌反应45min,反应结束后,抽滤,滤饼用去离子水洗涤至中性,于70℃下干燥12h后,再于400℃下煅烧30min后,冷却至室温,得到包覆玻璃微珠;硝酸锌的乙醇溶液由硝酸锌和乙醇按照1g:5mL混合而成;
步骤5、将5.8g包覆玻璃微珠和70mL乙醇加入圆底烧瓶中,超声分散20min后,加入1.4g偶联剂KH-590,搅拌反应3h后,加入0.7g甲基丙烯酸三氟乙酯、0.3g改性剂和0.2g安息香双甲醚,紫外灯照射下,搅拌反应40min,反应结束后,抽滤,滤饼用去离子水洗涤4次,最后于60℃烘箱中干燥至恒重,得到功能填料。
实施例3
本实施例制备一种功能填料,步骤如下:
步骤1、氮气保护下,将50mmol环氧氯丙烷、50mmol 3,5-二叔丁基-4-羟基苯甲醇和52.3mL二甲基亚砜加入三口烧瓶中,控制温度60℃,搅拌反应10min,然后加入氢氧化钾,回流反应5h,反应结束后,制得中间产物1,然后控制反应温度5℃,向三口烧瓶中滴加50mmol 4-氨基-1,2,2,6,6-五甲基哌啶,1h内滴加结束,滴加结束后升温至21℃,搅拌反应2h,反应结束后,过滤,滤液用去离子水洗涤,之后乙酸乙酯萃取,旋蒸去除乙酸乙酯,制得中间产物2,氢氧化钾的用量为3,5-二叔丁基-4-羟基苯甲醇质量的6%;
步骤2、将0.1mol中间产物2和0.3mol丙烯酸加入反应釜中,进行搅拌并加入浓硫酸,在温度为90℃的条件下,进行反应3h,反应结束后,加入去离子水洗涤,用乙酸乙酯萃取后,旋蒸去除乙酸乙酯,制得改性剂,浓硫酸的用量为中间产物2和丙烯酸总质量的4%;
步骤3、将中空玻璃微珠加入浓度0.3mol/L的氢氧化钠溶液中搅拌1.5h后,过滤,滤饼用蒸馏水洗涤至洗涤液呈中性,再于70℃烘箱中干燥至恒重,得到刻蚀玻璃微珠,其中中空玻璃微珠和氢氧化钠溶液的用量比为1g:30mL;
步骤4、将6.8g刻蚀玻璃微珠、30mL水和20mL乙醇加入圆底烧瓶中,频率50kHz下超声分散40min,然后加入5mL硝酸锌的乙醇溶液,搅拌10min后,加入0.6g氢氧化钠,室温搅拌反应60min,反应结束后,抽滤,滤饼用去离子水洗涤至中性,于70℃下干燥12h后,再于400℃下煅烧30min后,冷却至室温,得到包覆玻璃微珠;硝酸锌的乙醇溶液由硝酸锌和乙醇按照1g:5mL混合而成;
步骤5、将6.7g包覆玻璃微珠和80mL乙醇加入圆底烧瓶中,超声分散20min后,加入1.5g偶联剂KH-590,搅拌反应4h后,加入0.8g甲基丙烯酸三氟乙酯、0.4g改性剂和0.3g安息香双甲醚,紫外灯照射下,搅拌反应60min,反应结束后,抽滤,滤饼用去离子水洗涤5次,最后于60℃烘箱中干燥至恒重,得到功能填料。
对比例1
本对比例制备一种功能填料,步骤如下:
步骤1、将中空玻璃微珠加入浓度0.3mol/L的氢氧化钠溶液中搅拌1.5h后,过滤,滤饼用蒸馏水洗涤至洗涤液呈中性,再于70℃烘箱中干燥至恒重,得到刻蚀玻璃微珠,其中中空玻璃微珠和氢氧化钠溶液的用量比为1g:30mL;
步骤2、将6.7g刻蚀玻璃微珠和80mL乙醇加入圆底烧瓶中,超声分散20min后,加入1.5g偶联剂KH-550,搅拌反应4h后,抽滤,滤饼用去离子水洗涤5次,最后于60℃烘箱中干燥至恒重,得到功能填料。
实施例4
一种建筑用高耐候性密封胶的制备方法,包括以下步骤:
第一步、准备以下重量份原料:低聚物多元醇15份、HDI 5份、二羟甲基丙烯0.份、实施例1的功能填料3.7份、三乙胺0.1份、乙二醇0.5份、月桂酸二丁基锡0.01份、N-甲基吡咯烷酮3份、去离子水50份、增稠剂802B 0.5份;
第二步、将低聚物多元醇、HDI、二羟甲基丙烯、功能填料、月桂酸二丁基锡和N-甲基吡咯烷酮按照配方量加入反应釜中,升温至50℃,搅拌反应40min,得到第一混料;
第三步、将第一混料降温至20℃,加入乙二醇和去离子水,转速200r/min条件下,混合1h,最后加入三乙胺和增稠剂802B,搅拌1.5h,得到建筑用高耐候性密封胶。
其中,低聚物多元醇为聚己二酸丁二醇酯二元醇、聚碳酸酯二元醇、聚己内酯二元醇按照质量比1:1:1混合而成,数均分子量为1000。
实施例5
一种建筑用高耐候性密封胶的制备方法,包括以下步骤:
第一步、准备以下重量份原料:低聚物多元醇18份、HDI 8份、二羟甲基丙烯1.1份、实施例1的功能填料3.9份、三乙胺0.3份、乙二醇1.2份、月桂酸二丁基锡0.02份、N-甲基吡咯烷酮5份、去离子水70份、增稠剂802B 1.2份;
第二步、将低聚物多元醇、HDI、二羟甲基丙烯、功能填料、月桂酸二丁基锡和N-甲基吡咯烷酮按照配方量加入反应釜中,升温至80℃,搅拌反应50min,得到第一混料;
第三步、将第一混料降温至30℃,加入乙二醇和去离子水,转速250r/min条件下,混合1h,最后加入三乙胺和增稠剂802B,搅拌1.8h,得到建筑用高耐候性密封胶。
其中,低聚物多元醇为聚己二酸丁二醇酯二元醇、聚碳酸酯二元醇按照质量比1:1混合而成,数均分子量为2000。
实施例6
一种建筑用高耐候性密封胶的制备方法,包括以下步骤:
第一步、准备以下重量份原料:低聚物多元醇20份、HDI 13份、二羟甲基丙烯1.5份、实施例1的功能填料5.8份、三乙胺0.5份、乙二醇3.0份、月桂酸二丁基锡0.04份、N-甲基吡咯烷酮11份、去离子水80份、增稠剂802B 2份;
第二步、将低聚物多元醇、HDI、二羟甲基丙烯、功能填料、月桂酸二丁基锡和N-甲基吡咯烷酮按照配方量加入反应釜中,升温至90℃,搅拌反应60min,得到第一混料;
第三步、将第一混料降温至40℃,加入乙二醇和去离子水,转速300r/min条件下,混合1h,最后加入三乙胺和增稠剂802B,搅拌2.5h,得到建筑用高耐候性密封胶。
其中,低聚物多元醇为聚己二酸丁二醇酯二元醇、聚四氢呋喃醚二醇和聚四亚甲基醚二醇按照质量比1:1:1混合而成,数均分子量为3000。
对比例2
将实施例4中的功能粒子去除,其余原料及制备过程不变。
对比例3
将实施例5中的功能粒子替换为对比例1中的功能粒子,其余原料及制备过程不变。
对比例4
本对比例为衡水亚冠橡胶制品有限公司出售的单组分聚氨酯密封胶。
将实施例4-6和对比例2-4所得的密封胶进行性能测试,测试项目和标准如下:
硬度(邵尔硬度):采用上海市六菱仪器厂产LX-A型橡胶硬度计依据GB/T531.1-2008《硫化橡胶或热塑性橡胶压入硬度试验方法第一部分:邵氏硬度计法》进行测试
表干时间(h):依据GB/T13477.5-2017《建筑密封材料试验方法第5部分:表干时间的测定》进行测试。
下垂度(mm):采用选取万能拉力试验机,依据GB/T 13477.62002《建筑密封材料试验方法第6部分:流动性的测定》进行测试。
断裂伸长率(%):采用万能拉力试验机,依据GB/T13477.8-2017进行测试。
水-紫外线辐照后定伸性能60%:采用郑州惠冕材料科技有限公司产SZW-3型水-紫外线辐照控制仪,依据JG/T4852007《建筑窗用弹性密封胶》进行测试。
耐水性:将各组密封胶均匀涂布与钢板下,室温固化27h,养护7h后,在水中浸泡30d,观察有无脱落、气泡等变化;
耐酸性:将各组密封胶均匀涂布与钢板下,室温固化27h,养护7h后,在质量分数10%硫酸溶液中浸泡20d,观察有无脱落、气泡等变化;
耐碱性:将各组密封胶均匀涂布与钢板下,室温固化27h,养护7h后,在质量分数10%氢氧化钠溶液中中浸泡20d,观察有无脱落、气泡等变化。
测试结果如表1所示:
表1
由表1可以看出,实施例4-6的密封胶在硬度、表干时间、下垂度、断裂伸长率、抗紫外和耐水、耐酸碱测试过程中表现均匀优于对比例2-4,说明本发明制备的密封胶相比于市面上的密封胶,不仅使用方便,还具有优异的抗氧化、耐酸碱、防水性能。
将实施例4-6和对比例2-4所得的密封胶涂覆与水泥砂浆材质板体壁的表面,按照GB/T10295-2008,采用热流发导热仪进行隔热保温性能测试,测试结果如表2所示:
表2
项目 | 导热系数λW/(m,K) |
实施例4 | 0.021 |
实施例5 | 0.020 |
实施例6 | 0.021 |
对比例2 | 0.051 |
对比例3 | 0.036 |
对比例4 | 0.042 |
由表2可以看出,实施例4-6的密封胶的导热系数在0.020-0.021W/(m,K),均低于对比例2-4,说明本发明制备的密封胶具有较好的保温隔热性能,在建筑材料中具有很大的应用价值。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (8)
1.一种建筑用高耐候性密封胶的制备方法,其特征在于,包括以下步骤:
第一步、称取原料;
第二步、将低聚物多元醇、异氰酸酯单体、亲水改性剂、功能填料、催化剂和有机溶剂按照配方量加入反应釜中,升温至50-90℃,搅拌反应40-60min,得到第一混料;
第三步、将第一混料降温至20-40℃,加入扩链剂和去离子水混合后,加入pH调节剂和增稠剂,搅拌1.5-2.5h,得到建筑用高耐候性密封胶;
其中,功能填料由以下步骤制成:
将包覆玻璃微珠和乙醇超声分散,加入偶联剂KH-590,搅拌反应2-4h后,加入甲基丙烯酸三氟乙酯、改性剂和安息香双甲醚,紫外灯照射下,搅拌反应30-60min,反应结束后,抽滤,滤饼洗涤、干燥,得到功能填料。
2.根据权利要求1所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,第一步原料按重量份配比如下:
低聚物多元醇15-20份、异氰酸酯单体5-13份、亲水改性剂0.8-1.5份、功能填料3.7-5.8份、pH调节剂0.1-0.5份、扩链剂0.5-3.0份、催化剂0.01-0.04份、有机溶剂3-11份、去离子水50-80份、增稠剂0.5-2份。
3.根据权利要求1所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,改性剂由以下步骤制成:
步骤1、氮气保护下,将环氧氯丙烷、3,5-二叔丁基-4-羟基苯甲醇和二甲基亚砜混合,控制温度50-60℃,加入氢氧化钾,回流反应3-5h,制得中间产物1,控制温度0-5℃,滴加4-氨基-1,2,2,6,6-五甲基哌啶,滴加结束后升温至19-21℃,搅拌反应2h,过滤,滤液洗涤、萃取,旋蒸,制得中间产物2;
步骤2、将中间产物2和丙烯酸混合,加入浓硫酸,温度80-90℃下,反应2-3h,洗涤,萃取,旋蒸,制得改性剂。
4.根据权利要求3所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,步骤1中氢氧化钾的用量为3,5-二叔丁基-4-羟基苯甲醇质量的4-6%。
5.根据权利要求3所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,步骤2中浓硫酸的用量为中间产物2和丙烯酸总质量的2-4%。
6.根据权利要求1所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,包覆玻璃微珠由以下步骤制成:
将刻蚀玻璃微珠、水和乙醇超声分散,加入硝酸锌的乙醇溶液,室温搅拌后加入氢氧化钠,反应30-60min,抽滤,滤饼洗涤、干燥后于400℃下煅烧30min后,冷却至室温,得到包覆玻璃微珠。
7.根据权利要求6所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,刻蚀玻璃微珠由以下步骤制成:
将中空玻璃微珠加入氢氧化钠溶液中搅拌1.5h后,过滤,滤饼洗涤、干燥,得到刻蚀玻璃微珠。
8.根据权利要求1所述的一种建筑用高耐候性密封胶的制备方法,其特征在于,pH调节剂为三乙胺、醋酸和赖氨酸中的一种。
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