CN110591048A - 一种含氟水性环氧固化剂的制备方法 - Google Patents
一种含氟水性环氧固化剂的制备方法 Download PDFInfo
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- CN110591048A CN110591048A CN201910898674.0A CN201910898674A CN110591048A CN 110591048 A CN110591048 A CN 110591048A CN 201910898674 A CN201910898674 A CN 201910898674A CN 110591048 A CN110591048 A CN 110591048A
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- fluorine
- curing agent
- glycidyl ether
- epoxy curing
- epoxy resin
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- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 7
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- IYNGLSRZLOHZJA-UHFFFAOYSA-N 1,4,7-triazabicyclo[5.2.2]undecane Chemical compound C1CN2CCN1CCNCC2 IYNGLSRZLOHZJA-UHFFFAOYSA-N 0.000 claims description 3
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- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 3
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- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 6
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- HRWYHCYGVIJOEC-UHFFFAOYSA-N 2-(octoxymethyl)oxirane Chemical compound CCCCCCCCOCC1CO1 HRWYHCYGVIJOEC-UHFFFAOYSA-N 0.000 description 2
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明公开了一种含氟水性环氧固化剂的制备方法,涉及一种固化剂,首先采用多巴胺的自聚合反应在含氟聚合物微粉表面包覆一层聚多巴胺,对其进行功能化修饰,再与多异氰酸酯、聚醚多元醇、亲水扩链剂按一定比例反应,获得一端含异氰酸酯基的聚氨酯预聚体,然后加入环氧树脂,继续反应制备新型含氟聚氨酯预聚体接枝的环氧树脂;再将单环氧缩水甘油醚滴加到多乙烯多胺中,制备单封端的多乙烯多胺;最后将含氟聚氨酯预聚体接枝的环氧树脂滴加到单封端的多乙烯多胺中,反应获得柔韧性好、耐热性、耐碱性、耐磨性和耐水性的水性环氧固化剂。
Description
技术领域
本发明涉及一种固化剂,具体涉及一种含氟的水性环氧固化剂及其制备方法。
背景技术
环氧树脂具有绝缘性、机械强度高及安全健康方面等优势而被广泛应用于建筑、交通及化工等各个领域。同时对各种底材的适用性和极佳的涂膜性能、极强的附着力,能够在工业地坪和大型停车坪方面,在国内已经有很多成功的应用实例。但环氧树脂固化物存在质脆、耐冲击性差、容易开裂和耐水性不足等缺点,又限制了环氧树脂的进一步扩大应用,所以如何提高环氧树脂固化产物的综合性能具有重要意义。
常见的水性环氧树脂涂料多为由水性环氧树脂乳液和水性环氧固化剂所形成的,在环氧树脂固化剂中,胺类固化剂是用量最大且最广的环氧固化剂。当前的水性环氧固化剂多采用多乙烯多胺体系,但这类固化剂室温易挥发,毒性大,固化速度快及固化膜耐水性差,耐酸碱腐蚀性差,柔韧性差,难以满足社会发展对高性能涂料的需要,大大限制了其推广应用。随着人们对环境保护要求的日益严格以及固化剂的性质对涂膜的物理和化学性能影响,环氧涂料的水性化和功能化成为其发展的主要趋势。对传统的环氧固化剂进行改性,向其引入柔性韧性好的链段以及功能性基团,能够有效改善环氧固化剂,不仅克服了常规固化剂的缺点,增强涂膜的物理和化学性能,且环保无害,符合环保要求。
基于以上背景,制备性能优异且环保无害的水性环氧固化剂,与水性环氧乳液的相溶性好,可改善环氧固化膜的柔韧性、耐热性、耐酸碱性及耐摩性等特性,进一步扩大了环氧树脂涂料实际应用。
发明内容
本发明的目的在于克服现有技术的不足,提供了一种苯胺三聚体改性水性聚偏二氯乙烯重防腐涂料及其制备方法,以解决现有技术中水性环氧固化剂柔韧性、耐热性等较差的技术问题。
本发明是通过以下技术方案实现的:
本发明提供了一种含氟水性环氧固化剂的制备方法,包括以下步骤:
(1)功能化改性含氟聚合物微粉
将0.5-1.8g含氟聚合物微粉分散到含有500mL pH=8.5的Tris缓冲溶液中,磁力搅拌形成均匀悬浮液后,将0.1-0.3g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12-24h,通过重复离心、洗涤和干燥后,获得功能化改性含氟聚合物微粉;
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将40-60g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入20-40g多异氰酸酯,在0.1-0.2g催化剂作用下,反应温度控制在50~80℃,反应时间为1.5~2.5h;再加入2-3g亲水扩链剂,控制温度在70~85℃继续反应1~2h;加入1-2g步骤1的产物,控制温度在70~85℃,反应1.5~2h;再加入40-60g环氧树脂E-51,升温至70~90℃,反应1.5~3h,获得含氟聚氨酯预聚体接枝的环氧树脂;
(3)制备单封端多乙烯多胺
将单环氧缩水甘油醚缓慢滴入到多乙烯多胺,单环氧缩水甘油醚与多乙烯多胺的摩尔比为1.1:1,反应温度为60~80℃,反应时间为3~4h,获得单封端多乙烯多胺;
(4)制备含氟水性环氧固化剂
将50-60g步骤3的产物和溶剂缓慢滴加到60-80g步骤2中,用量比为1:1-1:1.5,控制温度在60-80℃下反应3-4h,随后加入10-15g乙酸成盐,于55-65℃下继续反应0.5-1小时,反应结束后减压蒸馏除去溶剂,加入去离子水,制得含氟水性环氧固化剂,固含量控制在45-55%。
进一步,所述含氟聚合物微粉为聚四氟乙烯、聚偏氟乙烯、聚氟乙烯、聚三氟氯乙烯的一种或共混物。
进一步,所述聚醚多元醇为聚醚二元醇,其平均分子量1000-4000。
进一步,所述多异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、二苯基甲烷二异氰酸酯(MDI)、二聚酸二异氰酸酯(DDI)中的一种或共混物。
进一步,所述催化剂为二月桂酸二丁基锡或辛酸亚锡。
进一步,所述亲水扩链剂含羧酸、磺酸、磷酸基团中的一种基团,选自二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)、2-[(2-氨乙基)氨基]磺酸钠中的至少一种
进一步,所述单环氧缩水甘油醚为叔碳酸甘油醚、苄基缩水甘油醚、烯丙基缩水甘油醚、丁基缩水甘油醚、苯基缩水甘油醚、C12-14缩水甘油醚中的一种或共混物。
进一步,所述多乙烯多胺为三乙烯二胺、四乙烯三胺或五乙烯四胺。
进一步,所述溶剂为丙二醇甲醚、丙二醇乙醚、乙二醇乙醚中的一种或共混物。
与现有技术相比,本发明具有以下优点:
本发明的一种含氟水性环氧固化剂的制备方法,其制备获得的固化剂与常规含氟环氧固化剂相比,常规含氟环氧固化剂通过接枝含氟化合物单体,工艺复杂且产物转化率不高,而掺杂功能化改性的聚四氟乙烯微粉,与环氧固化剂相容好、工艺简单,可改善环氧固化膜所不具有的性能,极大增强环氧树脂固化膜应用范围。
进一步,本发明通过聚氨酯预聚体改性环氧固化剂,能够兼具聚氨酯和环氧树脂两者特性,同时将含氟树脂引入固化剂中,使该固化膜具有高硬度、柔韧性好、耐磨性好、较低的导电性、优异的表面性能,同时满足人们对于涂料环保无害的要求。
附图说明
图1本发明提供的含氟水性环氧固化剂的制备方法的制备过程示意图。
具体实施方式
下面将结合本发明实施例中的附图,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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
结合图1,本发明按照以下方法制备含氟水性环氧固化剂:
一种含氟水性环氧固化剂的制备方法,包括以下步骤:
(1)功能化改性含氟聚合物微粉
将0.5-1.8g含氟聚合物微粉分散到含有500mL pH=8.5的Tris缓冲溶液中,磁力搅拌形成均匀悬浮液后,将0.1-0.3g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12-24h,通过重复离心、洗涤和干燥后,获得功能化改性含氟聚合物微粉;
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将40-60g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入20-40g多异氰酸酯,在0.1-0.2g催化剂作用下,反应温度控制在50~80℃,反应时间为1.5~2.5h;再加入2-3g亲水扩链剂,控制温度在70~85℃继续反应1~2h;加入1-2g步骤1的产物,控制温度在70~85℃,反应1.5~2h;再加入40-60g环氧树脂E-51,升温至70~90℃,反应1.5~3h,获得含氟聚氨酯预聚体接枝的环氧树脂;
(3)制备单封端多乙烯多胺
将单环氧缩水甘油醚缓慢滴入到多乙烯多胺,单环氧缩水甘油醚与多乙烯多胺的摩尔比为1.1:1,反应温度为60~80℃,反应时间为3~4h,获得单封端多乙烯多胺;
(4)制备含氟水性环氧固化剂
将50-60g步骤3的产物和溶剂缓慢滴加到60-80g步骤2中,用量比为1:1-1:1.5,控制温度在60-80℃下反应3-4h,随后加入10-15g乙酸成盐,于55-65℃下继续反应0.5-1小时,反应结束后减压蒸馏除去溶剂,加入去离子水,制得含氟水性环氧固化剂,固含量控制在45-55%。
特别的,所述含氟聚合物微粉为聚四氟乙烯、聚偏氟乙烯、聚氟乙烯、聚三氟氯乙烯的一种或共混物。
特别的,所述聚醚多元醇为聚醚二元醇,其平均分子量1000-4000。
特别的,所述多异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、二苯基甲烷二异氰酸酯(MDI)、二聚酸二异氰酸酯(DDI)中的一种或共混物。
特别的,所述催化剂为二月桂酸二丁基锡或辛酸亚锡。
特别的,所述亲水扩链剂含羧酸、磺酸、磷酸基团中的一种基团,选自二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)、2-[(2-氨乙基)氨基]磺酸钠中的至少一种
特别的,所述单环氧缩水甘油醚为叔碳酸甘油醚、苄基缩水甘油醚、烯丙基缩水甘油醚、丁基缩水甘油醚、苯基缩水甘油醚、C12-14缩水甘油醚中的一种或共混物。
特别的,所述多乙烯多胺为三乙烯二胺、四乙烯三胺或五乙烯四胺。
特别的,所述溶剂为丙二醇甲醚、丙二醇乙醚、乙二醇乙醚中的一种或共混物。
以下为本发明按照上述方法提供的具体实施例
实例一
一种含氟水性环氧固化剂的制备方法,包括如下步骤:
(1)功能化改性含氟聚合物微粉
将0.86g含氟聚合物微粉分散到含有500毫升的Tris缓冲溶液(pH=8.5)中,磁力搅拌形成均匀悬浮液后,将0.12g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12小时,通过重复离心、洗涤、干燥等过程,获得功能化改性含氟聚合物微粉。
特别的,在本实施例中含氟聚合物微粉具体为聚四氟乙烯。
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将50g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入22.2g IPDI以及0.1g辛酸亚锡,反应温度控制在80℃,反应时间为2.5h;再加入2.2g DMPA,控制温度在85℃继续反应1.5h;加入步骤1产物,控制温度在85℃,反应2h;再加入40g环氧树脂E-51,升温至90℃,反应2.5h,获得含氟聚氨酯预聚体接枝的环氧树脂。
(3)制备单封端四乙烯五胺
将102g辛基缩水甘油醚缓慢滴入到95g四乙烯五胺,辛基缩水甘油醚与四乙烯五胺的摩尔比为1.1:1.0,反应温度为70℃,反应时间为3h,获得单封端四乙烯五胺。
(4)制备含氟水性环氧固化剂
将51g步骤3制备的单封端四乙烯五胺缓慢滴加到62g步骤2制备的含氟聚氨酯预聚体接枝的环氧树脂和45g丙二醇甲醚中,控制温度在80℃下反应3h,随后加入10.8g乙酸成盐,于55℃下继续反应0.5h,反应结束后减压蒸馏除去溶剂,加入去离子水,制得新型含氟水性环氧树脂固化剂,固含量为53%。
将上述的含氟水性环氧固化剂与水性环氧树脂按比例混合,配制比例如下:
组分A:E-51 45g
组分B:实例1所得含氟水性环氧固化剂 100g
将两组分混合均匀,在室温条件下固化成膜,固化膜性能检测如表1:
检测项目 | 检测结果 | 检验方法 |
热分解温度/℃ | 316 | GB/T 30711-2014 |
铅笔硬度 | 3H | GB/T 6739-2006 |
附着力/级 | 1 | GB/T 1720-79 |
柔韧性/mm | 1 | GB/T 1731-93 |
耐冲击性/KJ/m<sup>2</sup> | 23.4 | GB/T 1732-93 |
耐水性/7d | 无明显变化 | GB/T 1733-93 |
耐碱性/30d | 无明显变化 | GB/T 9256-2009 |
表1
实例二
一种含氟水性环氧固化剂的制备方法,包括如下步骤:
(1)功能化改性含氟聚合物微粉
将1.52g聚偏氟乙烯分散到含有500毫升的Tris缓冲溶液(pH=8.5)中,磁力搅拌形成均匀悬浮液后,将0.26g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌24小时,通过重复离心、乙醇和去离子水洗涤、干燥等过程,获得功能化改性的含氟聚合物微粉。
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将50g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入32.7g TDI以及0.1g二月桂酸二丁基锡,反应温度控制在80℃,反应时间为2.5h;再加入2.8g DMBA,控制温度在85℃继续反应1.5h;加入步骤1的产物,控制温度在85℃,反应2h;再加入60g环氧树脂E-51,升温至90℃,反应2.5h。
(3)制备单封端多乙烯多胺
将102g苄基缩水甘油醚缓慢滴入到95g三乙烯二胺,反应温度为70℃,反应时间为3h。
(4)制备含氟水性环氧固化剂
将60g步骤3制备的单封端多乙烯多胺缓慢滴加到72g步骤2制备新型含氟聚氨酯预聚体接枝的环氧树脂和45g丙二醇乙醚中,控制温度在80℃下反应3h,随后加入11.9g乙酸成盐,于55℃下继续反应0.5h,反应结束后减压蒸馏除去溶剂,加入去离子水,制得新型含氟水性环氧树脂固化剂,固含量为52.5%。
将上述的含氟水性环氧固化剂与水性环氧树脂按比例混合,配制比例如下:
组分A:E-51 53g
组分B:实例2所得含氟水性环氧固化剂 100g
将两组分混合均匀,在室温条件下固化成膜,固化膜性能检测如表2:
检测项目 | 检测结果 | 检验方法 |
热分解温度/℃ | 335 | GB/T 30711-2014 |
铅笔硬度 | 4H | GB/T 6739-2006 |
附着力/级 | 1 | GB/T 1720-79 |
柔韧性/mm | 1 | GB/T 1731-93 |
耐冲击性/KJ/m<sup>2</sup> | 24.3 | GB/T 1732-93 |
耐水性/7d | 无明显变化 | GB/T 1733-93 |
耐碱性/30d | 无明显变化 | GB/T 9256-2009 |
表2
实例三
一种含氟水性环氧固化剂的制备方法,包括如下步骤:
(1)功能化改性含氟聚合物微粉
将1.52g聚氟乙烯分散到含有500毫升的Tris缓冲溶液(pH=8.5)中,磁力搅拌形成均匀悬浮液后,将0.26g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12-24小时,通过重复离心、乙醇和去离子水洗涤、干燥等过程,获得功能化改性的含氟聚合物微粉。
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将40g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入37g DDI以及0.3g辛酸亚锡,反应温度控制在85℃,反应时间为2.5h;再加入2.8g 2-[(2-氨乙基)氨基]磺酸钠,控制温度在85℃继续反应1.5h;加入步骤1的产物,控制温度在85℃,反应2h;再加入60g环氧树脂E-51,升温至90℃,反应2.5h。
(3)制备单封端多乙烯多胺
将102g丁基缩水甘油醚缓慢滴入到95g五乙烯四胺,反应温度为70℃,反应时间为3h。
(4)制备含氟水性环氧固化剂
将58g步骤3制备的单封端多乙烯多胺缓慢滴加到69g步骤2制备新型含氟聚氨酯预聚体接枝的环氧树脂和45g乙二醇乙醚中,控制温度在80℃下反应3h,随后加入12.7g乙酸成盐,于55℃下继续反应0.5h,反应结束后减压蒸馏除去溶剂,加入去离子水,制得新型含氟水性环氧树脂固化剂,固含量为53%。
将上述的含氟水性环氧固化剂与水性环氧树脂按比例混合,配制比例如下:
组分A:E-51 55g
组分B:实例2所得含氟水性环氧固化剂 100g
将两组分混合均匀,在室温条件下固化成膜,固化膜性能检测如表3:
检测项目 | 检测结果 | 检验方法 |
热分解温度/℃ | 322 | GB/T 30711-2014 |
铅笔硬度 | 4H | GB/T 6739-2006 |
附着力/级 | 1 | GB/T 1720-79 |
柔韧性/mm | 1 | GB/T 1731-93 |
耐冲击性/KJ/m<sup>2</sup> | 23.8 | GB/T 1732-93 |
耐水性/7d | 无明显变化 | GB/T 1733-93 |
耐碱性/30d | 无明显变化 | GB/T 9256-2009 |
表3
实例四
一种含氟水性环氧固化剂的制备方法,包括如下步骤:
(1)功能化改性含氟聚合物微粉
将1.52g聚三氟氯乙烯分散到含有500毫升的Tris缓冲溶液(pH=8.5)中,磁力搅拌形成均匀悬浮液后,将0.26g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12-24小时,通过重复离心、乙醇和去离子水洗涤、干燥等过程,获得功能化改性的含氟聚合物微粉。
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将60g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入22.2g MDI以及0.1g二月桂酸二丁基锡,反应温度控制在80℃,反应时间为2.5h;再加入2.2g DMPA,控制温度在85℃继续反应1.5h;加入步骤1的产物,控制温度在85℃,反应2h;再加入40g环氧树脂E-51,升温至90℃,反应2.5h。
(3)制备单封端多乙烯多胺
将102gC12-14缩水甘油醚缓慢滴入到95g四乙烯五胺,反应温度为70℃,反应时间为3h。
(4)制备含氟水性环氧固化剂,将52g步骤3制备的单封端多乙烯多胺缓慢滴加到70g步骤2制备新型含氟聚氨酯预聚体接枝的环氧树脂和45g丙二醇甲醚中,控制温度在80℃下反应3h,随后加入11.2g乙酸成盐,于55℃下继续反应0.5h,反应结束后减压蒸馏除去溶剂,加入去离子水,制得新型含氟水性环氧树脂固化剂,固含量为54.5%。
将上述的含氟水性环氧固化剂与水性环氧树脂按比例混合,配制比例如下:
组分A:E-51 49g
组分B:实例2所得含氟水性环氧固化剂 100g
将两组分混合均匀,在室温条件下固化成膜,固化膜性能检测如表4::
检测项目 | 检测结果 | 检验方法 |
热分解温度/℃ | 301 | GB/T 30711-2014 |
铅笔硬度 | 3H | GB/T 6739-2006 |
附着力/级 | 1 | GB/T 1720-79 |
柔韧性/mm | 1 | GB/T 1731-93 |
耐冲击性/KJ/m<sup>2</sup> | 22.9 | GB/T 1732-93 |
耐水性/7d | 微泛白 | GB/T 1733-93 |
耐碱性/30d | 起泡 | GB/T 9256-2009 |
表4
由实施例1-4可以看出,本发明提供的聚氨酯预聚体改性环氧固化剂,能够兼具聚氨酯和环氧树脂两者特性,同时将含氟树脂引入固化剂中,使该固化膜具有高硬度、柔韧性好、耐磨性好、较低的导电性、优异的表面性能,同时满足人们对于涂料环保无害的要求
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 (9)
1.一种含氟水性环氧固化剂的制备方法,其特征在于,包括以下步骤:
(1)功能化改性含氟聚合物微粉
将0.5-1.8g含氟聚合物微粉分散到含有500mL pH=8.5的Tris缓冲溶液中,磁力搅拌形成均匀悬浮液后,将0.1-0.3g多巴胺加入悬浮液中,并将其混合物在室温下轻微磁力搅拌12-24h,通过重复离心、洗涤和干燥后,获得功能化改性含氟聚合物微粉;
(2)制备含氟聚氨酯预聚体接枝的环氧树脂
将40-60g聚四氢呋喃二醇加热抽真空120℃脱水2h,降温至50℃,加入20-40g多异氰酸酯,在0.1-0.2g催化剂作用下,反应温度控制在50~80℃,反应时间为1.5~2.5h;再加入2-3g亲水扩链剂,控制温度在70~85℃继续反应1~2h;加入1-2g步骤1的产物,控制温度在70~85℃,反应1.5~2h;再加入40-60g环氧树脂E-51,升温至70~90℃,反应1.5~3h,获得含氟聚氨酯预聚体接枝的环氧树脂;
(3)制备单封端多乙烯多胺
将单环氧缩水甘油醚缓慢滴入到多乙烯多胺,单环氧缩水甘油醚与多乙烯多胺的摩尔比为1.1:1,反应温度为60~80℃,反应时间为3~4h,获得单封端多乙烯多胺;
(4)制备含氟水性环氧固化剂
将50-60g步骤3的产物和溶剂缓慢滴加到60-80g步骤2中,用量比为1:1-1:1.5,控制温度在60-80℃下反应3-4h,随后加入10-15g乙酸成盐,于55-65℃下继续反应0.5-1小时,反应结束后减压蒸馏除去溶剂,加入去离子水,制得含氟水性环氧固化剂,固含量控制在45-55%。
2.根据权利要求1所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述含氟聚合物微粉为聚四氟乙烯、聚偏氟乙烯、聚氟乙烯、聚三氟氯乙烯的一种或共混物。
3.根据权利要求2所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述聚醚多元醇为聚醚二元醇,其平均分子量1000-4000。
4.根据权利要求3所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述多异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、甲苯二异氰酸酯(TDI)、六亚甲基二异氰酸酯(HDI)、二苯基甲烷二异氰酸酯(MDI)、二聚酸二异氰酸酯(DDI)中的一种或共混物。
5.根据权利要求4所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述催化剂为二月桂酸二丁基锡或辛酸亚锡。
6.根据权利要求5所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述亲水扩链剂含羧酸、磺酸、磷酸基团中的一种基团,选自二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)、2-[(2-氨乙基)氨基]磺酸钠中的至少一种。
7.根据权利要求6所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述单环氧缩水甘油醚为叔碳酸甘油醚、苄基缩水甘油醚、烯丙基缩水甘油醚、丁基缩水甘油醚、苯基缩水甘油醚、C12-14缩水甘油醚中的一种或共混物。
8.根据权利要求7所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述多乙烯多胺为三乙烯二胺、四乙烯三胺或五乙烯四胺。
9.根据权利要求8所述的一种含氟水性环氧固化剂的制备方法,其特征在于,所述溶剂为丙二醇甲醚、丙二醇乙醚、乙二醇乙醚中的一种或共混物。
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