CN114539503A - 一种织物涂层用阻燃聚氨酯树脂及其制备方法 - Google Patents
一种织物涂层用阻燃聚氨酯树脂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种织物涂层用阻燃聚氨酯树脂及其制备方法,该阻燃聚氨酯树脂的原料配方包括以下组分:聚酯多元醇和/或聚醚多元醇20~30%;反应型阻燃剂3~5%;反应型协效阻燃剂3~5%;异氰酸酯10~15%;扩链剂2~3%;溶剂50~55%;稳定剂0.001~0.01%;封端剂0.01~0.1%,反应型阻燃剂为无卤乙基磷酸酯齐聚物二元醇;反应型协效阻燃剂为含有Si‑OH官能团的羟基改性有机硅中间体。本发明通过采用聚酯多元醇和/或聚醚多元醇的多元醇组分,配合特定反应型阻燃剂和反应型协效阻燃剂及其他物质制备的聚氨酯树脂,用于织物涂层,不仅具有持久、优异的阻燃效果,同时保持了原有的粘接强度和弹性。
Description
技术领域
本发明属于织物涂层用聚氨酯树脂技术领域,具体涉及一种织物涂层用阻燃聚氨酯树脂及其制备方法。
背景技术
织物涂层是在机织或者针织面料表面涂覆一层均匀的覆盖胶料,从而达到防水、防风保暖、阻燃等功能。针对织物涂层不同用途对于涂层料有不同要求,例如耐水压、透湿、遮光、亮面等,广泛用于帐篷、服装、沙发、雨伞等。随着人们对环保及安全意识的提高,织物涂层的阻燃性也越来越被人们所重视。
现有技术中,通常是在覆盖胶料中通过后添加含卤、磷等阻燃剂,如三氧化二锑,能够提高织物产品的阻燃性,但是影响织物涂层的手感,并且阻燃成分会迁移至涂层表面,水洗后阻燃性能降低。
发明内容
本发明目的是为了克服现有技术的不足而提供一种织物涂层用阻燃聚氨酯树脂及其制备方法,将该阻燃聚氨酯树脂用于织物涂层,使得织物涂层具有持久且优异的阻燃效果同时具有优异的粘接强度和弹性。
为达到上述目的,本发明所采用的技术方案为:
一种织物涂层用阻燃聚氨酯树脂,按重量百分含量计,所述阻燃聚氨酯树脂的原料配方包括以下组分:
所述反应型阻燃剂为无卤乙基磷酸酯齐聚物二元醇;
所述反应型协效阻燃剂为含有Si-OH官能团的羟基改性有机硅中间体。
在一些优选实施方式中,按重量百分含量计,所述阻燃聚氨酯树脂的原料配方包括以下组分:
优选地,所述反应型阻燃剂的数均分子量为600~800。如所述反应型阻燃剂选自德国科莱恩公司的OP-550。
优选地,所述反应型协效阻燃剂的数均分子量为3000~4000。如所述反应型协效阻燃剂选自广州斯洛柯公司的Silok8814、Silok8865H,其硅含量大致为85%左右。
所述反应型协效阻燃剂采用含有Si-OH官能团的改性有机硅与反应型阻燃剂协同增效,相比传统的后添加型协效阻燃剂(如三氧化二锑),不仅能够获得持久且更优异的阻燃效果,还具有更加优异的粘接强度。
在一些实施方面,所述聚酯多元醇为由己二酸(AA)、对苯二甲酸(PTA)中的一种或两种与乙二醇(EG)、二乙二醇(DEG)、1,4-丁二醇(1,4-BG)中的一种或多种进行酯化反应制得的数均分子量为1500~2500的聚酯多元醇。
本发明中,利用聚酯多元醇和聚醚多元醇进行复配能够获得优异的综合性能,进一步地,聚酯多元醇采用带有苯环结构的聚酯多元醇,相比脂肪族聚酯多元醇能够获得更加优异的阻燃性能。
优选地,所述聚酯多元醇为由己二酸和对苯二甲酸与乙二醇、二乙二醇、1,4-丁二醇中的一种或多种进行酯化反应制得的聚酯多元醇。
在一些实施方面,所述聚醚多元醇为聚四亚甲基醚二醇(PTMEG)。优选地,所述聚醚多元醇的数均分子量为1500~2500。
根据本发明的一些实施方面,所述异氰酸酯为二苯基甲烷二异氰酸酯(MDI)。
根据本发明的一些实施方面,所述扩链剂为1,4-丁二醇、乙二醇中的一种或二者的组合。
根据本发明的一些实施方面,所述封端剂为甲醇。
根据本发明的一些实施方面,所述稳定剂为磷酸。
根据本发明的一些实施方面,所述溶剂为N,N-二甲基甲酰胺(DMF)、甲苯(TOL)中的一种或多种的组合。
根据本发明的一些实施方面,所述阻燃聚氨酯树脂的原料配方还包括0.01~0.1%抗氧剂。
本发明采取的第二技术方案:一种上述所述的织物涂层用阻燃聚氨酯树脂的制备方法,所述制备方法包括使聚酯多元醇、聚醚多元醇、反应型协效阻燃剂、稳定剂和一部分异氰酸酯在75±3℃下进行反应,然后降温至60~65℃,加入反应型阻燃剂进行反应,然后加入一部分溶剂和扩链剂降温,待温度降至55℃以下,加入剩余部分异氰酸酯,升温至70±5℃进行反应,反应至粘度60~80Pa.S/25℃,加入封端剂和剩余部分溶剂进行封端,制得所述阻燃聚氨酯树脂。
进一步地,所述反应型阻燃剂的加入按多次分批加入体系进行反应。所述反应型阻燃剂多次分批的方式加入,避免反应难以控制,并且要在反应后期加。所述反应型阻燃剂在反应前期加入,或者一次性加入,反应都难以控制,容易出现凝胶现象。
进一步地,所述一部分异氰酸酯按NCO:OH的摩尔比为1.8~2.2进行投料。
进一步地,所述一部分溶剂占所述溶剂总质量的50~55%进行投料。
进一步地,所述在75±3℃下进行反应1~3h;和/或,所述加入反应型阻燃剂份分2~4次加入体系,相邻两次间隔20~40min,所述反应型阻燃剂加入完毕,保持60~65℃反应0.5~1.5h;和/或,所述加入封端剂和剩余部分溶剂后反应5~7h。
由于上述技术方案运用,本发明与现有技术相比具有下列优点:
本发明通过采用聚酯多元醇和/或聚醚多元醇的多元醇组分,配合特定反应型阻燃剂和反应型协效阻燃剂及其他物质制备的聚氨酯树脂,用于织物涂层,不仅具有持久、优异的阻燃效果,同时保持了原有的粘接强度和弹性。
本发明阻燃聚氨酯树脂的制备方法先是将多元醇组分、反应型协效阻燃剂和一部分异氰酸酯先进行反应,降温后加入分次加入反应型阻燃剂,避免反应难以控制,然后进行扩链后再与异氰酸酯进行反应,然后进行封端。制备过程中,反应易于控制,不易凝胶,制备得到的聚氨酯树脂粘度较低,流动性好,用于织物涂层时,采用溶剂稀释后易于涂布。
具体实施方式
下面结合具体实施例对本发明的具体实施作进一步详细说明,但本发明的实施和保护范围不限于此。
以下实施例中,部分原料来源如下:
反应型阻燃剂:无卤乙基磷酸酯齐聚物二元醇,来源于德国科莱恩公司,型号OP-550。
反应型协效阻燃剂:含有Si-OH官能团的羟基改性有机硅中间体,来源于广州斯洛柯公司,型号Silok8814。
实施例1
本实施例提供的织物涂层用阻燃聚氨酯树脂,通过以下方法制备得到:
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、35g含有Si-OH官能团的羟基改性有机硅中间体(分子量3200)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95g MDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(分子量660),保持温度60~65℃反应1hr,再加入200g DMF和100g TOL并加入扩链剂15g 1,4-BG和10g EG,待温度降至60℃以下,加入50gMDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
本例中,聚酯多元醇为由己二酸(AA)、对苯二甲酸与乙二醇(EG)、二乙二醇(DEG)进行酯化反应制得的数均分子量为2000的聚酯多元醇,且己二酸和对苯二甲酸的投料摩尔比为1.5:1。
实施例2
本实施例提供的织物涂层用阻燃聚氨酯树脂,通过以下方法制备得到:
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、35g含有Si-OH官能团的羟基改性有机硅中间体(分子量3200)、0.02g磷酸、0.5g I-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(分子量660),保持温度60~65℃反应1hr,再加入200gDMF和100gTOL并加入扩链剂15g 1.4-BG和10g EG,待温度降至60℃以下,加入50g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260gDMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
本例中,聚酯多元醇为由己二酸与乙二醇(EG)、二乙二醇进行酯化反应制得的数均分子量为2000的聚酯多元醇。
实施例3
本实施例提供的织物涂层用阻燃聚氨酯树脂,通过以下方法制备得到:
将240g聚酯多元醇、35g含有Si-OH官能团的羟基改性有机硅中间体(3200分子量)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(660分子量),保持温度60~65℃反应1hr,再加入200g DMF和100gTOL并加入扩链剂15g1.4-BG和10gEG,待温度降至60℃以下,加入50g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
本例中,选用的聚酯多元醇同实施例1。
实施例4
本实施例提供的织物涂层用阻燃聚氨酯树脂,通过以下方法制备得到:
将240g聚醚多元醇(具体为PTMEG-2000)、35g含有Si-OH官能团的羟基改性有机硅中间体(3200分子量)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(660分子量),保持温度60~65℃反应1hr,再加入200g DMF和100gTOL并加入扩链剂30g1.4-BG,待温度降至60℃以下,加入55g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
对比例1
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:将实施例1中的无卤乙基磷酸酯齐聚物二元醇换成含溴聚酯多元醇。
本例的阻燃聚氨酯树脂通过以下方法制备得到:
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、35g含有Si-OH官能团的羟基改性有机硅中间体(分子量3200)、38克含溴聚酯多元醇(分子量为1000)、0.02g磷酸、0.5g I-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将94gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温2h,然后再加入200g DMF和100gTOL并加入扩链剂15g 1,4-BG和10gEG,待温度降至60℃以下,加入52g MDI,缓慢升温至75℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260gDMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
对比例2
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:将实施例1中的含有Si-OH官能团的羟基改性有机硅中间体换成三氧化二锑。
本例的阻燃聚氨酯树脂通过以下方法制备得到:
将130g聚酯多元醇、130g聚醚多元醇(具体为PTMEG-2000)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将90gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,均分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(分子量660),保持温度60~65℃反应1hr,再加入200g DMF和100g TOL并加入扩链剂15g 1,4-BG和10g EG,待温度降至60℃以下,加入50g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,搅拌30分钟后加入32g三氧化二锑,并充分搅拌1小时,冷却出料,包装称重。
对比例3
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:不加实施例1中的含有Si-OH官能团的羟基改性有机硅中间体。
本例的阻燃聚氨酯树脂通过以下方法制备得到:
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将85gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(分子量660),保持温度60~65℃反应1hr,再加入180g DMF和100gTOL并加入扩链剂15g1.4-BG和10gEG,待温度降至60℃以下,加入45g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
对比例4
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:不添加含有Si-OH官能团的羟基改性有机硅中间体和无卤乙基磷酸酯齐聚物二元醇。
将150g聚酯多元醇、150g聚醚多元醇(具体为PTMEG-2000)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将78gMDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后加入200g DMF和100g TOL并加入扩链剂17g 1,4-BG和14g EG,待温度降至60℃以下,加入63gMDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重
对比例5
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:用双端羟乙基硅油代替含有Si-OH官能团的羟基改性有机硅中间体,本例中,双端羟乙基硅油为山东大易化工有限公司的DY-OH503羟基硅油。
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、38g含有Si-OH官能团的双端羟乙基硅油(分子量2000)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95g MDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g无卤乙基磷酸酯齐聚物二元醇(分子量660),保持温度60~65℃反应1hr,再加入200g DMF和100g TOL并加入扩链剂15g 1,4-BG和10g EG,待温度降至60℃以下,加入50g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260gDMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
本例中,聚酯多元醇为由己二酸(AA)、对苯二甲酸与乙二醇(EG)、二乙二醇(DEG)进行酯化反应制得的数均分子量为2000的聚酯多元醇,且己二酸和对苯二甲酸的投料摩尔比为1.5:1。
对比例6
本对比例提供的织物涂层用阻燃聚氨酯树脂,与实施例1的不同之处在于:用三(一缩二丙二醇)亚磷酸酯代替无卤乙基磷酸酯齐聚物二元醇。
将120g聚酯多元醇、120g聚醚多元醇(具体为PTMEG-2000)、35g含有Si-OH官能团的羟基改性有机硅中间体(分子量3200)、0.02g磷酸、0.5gI-1010加入反应釜中,进行充分搅拌均匀,温度控制在50℃,搅拌时间为40min,然后将95g MDI按NCO:OH的摩尔比为2.0加入反应釜,控制温度缓慢升温至75℃,并恒温1.5h,然后降温至65℃,分三次(间隔30分钟)加入36g三(一缩二丙二醇)亚磷酸酯,保持温度60~65℃反应1hr,再加入200g DMF和100gTOL并加入扩链剂15g 1,4-BG和10g EG,待温度降至60℃以下,加入50g MDI,缓慢升温至70℃,反应至粘度为60~80Pa.S/75℃,然后加入0.2g甲醇和260g DMF进行封端反应,反应时间为6小时,冷却出料,包装称重。
本例中,聚酯多元醇为由己二酸(AA)、对苯二甲酸与乙二醇(EG)、二乙二醇(DEG)进行酯化反应制得的数均分子量为2000的聚酯多元醇,且己二酸和对苯二甲酸的投料摩尔比为1.5:1。
将实施例1~4和对比例1~6制备的阻燃聚氨酯树脂,按聚氨酯树脂与甲苯溶剂以质量比100:30进行复配,然后涂布于牛津布上,制得织物样品,然后对织物样品进行性能测试,结果如表1和2所示。
表1为采用实施例1~4制备的阻燃聚氨酯树脂制备的织物涂层的性能测试结果
表2为采用对比例1~6制备的阻燃聚氨酯树脂制备的织物涂层的性能测试结果
表中各项性能测试的方法:
阻燃测试:垂直点燃,比较离开火焰后熄灭时间以及发烟量。
伸长率:拉力机测试,依据标准ISO1184-1983《塑料薄膜拉伸性能的测定》。
拉伸强度:拉力机测试,依据标准ISO1184-1983《塑料薄膜拉伸性能的测定》。
剥离强度:将3cm宽、12cm长热熔胶布条热压到涂层表面,留取2cm长,沿热熔胶布条裁取测试样,将留取的2cm长织物涂层和热熔胶布条分别用拉力机夹具夹住,启动拉力机测试。依据标准FZ/T 01010-2012《中华人民共和国纺织行业标准》。
模量:拉力机测试,依据标准ISO1184-1983《塑料薄膜拉伸性能的测定》。
由表1和表2的结果可见,采用无卤乙基磷酸酯齐聚物二元醇搭配硅含量85%左右的含有Si-OH官能团的羟基改性有机硅中间体制备的聚氨酯树脂,用于织物涂层上,能达到优异的阻燃且无烟性能,而含有苯环结构的聚酯多元醇对阻燃性能有所提高,并且采用本申请特定的反应型阻燃剂和反应型协效阻燃剂配合使用,剥离强度较高,伸长率和拉伸强度均较高,保持了原有的粘接强度和弹性。
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。
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值,这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说,各个范围的端点值之间、各个范围的端点值和单独的点值之间,以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围,这些数值范围应被视为在本文中具体公开。
Claims (10)
3.根据权利要求1或2所述的织物涂层用阻燃聚氨酯树脂,其特征在于:所述反应型阻燃剂的数均分子量为600~800;和/或,所述反应型协效阻燃剂的数均分子量为3000~4000。
4.根据权利要求3所述的织物涂层用阻燃聚氨酯树脂,其特征在于:所述反应型阻燃剂选自德国科莱恩公司的OP-550;和/或,所述反应型协效阻燃剂选自广州斯洛柯公司的Silok8814、Silok8865H。
5.根据权利要求1或2所述的织物涂层用阻燃聚氨酯树脂,其特征在于:所述聚酯多元醇为由己二酸、对苯二甲酸中的一种或两种与乙二醇、二乙二醇、1,4-丁二醇中的一种或多种进行酯化反应制得的数均分子量为1500~2500的聚酯多元醇;和/或,所述聚醚多元醇为聚四亚甲基醚二醇。
6.根据权利要求5所述的织物涂层用阻燃聚氨酯树脂,其特征在于:所述聚酯多元醇为由己二酸和对苯二甲酸与乙二醇、二乙二醇、1,4-丁二醇中的一种或多种进行酯化反应制得的聚酯多元醇;和/或,所述聚醚多元醇的数均分子量为1500~2500。
7.根据权利要求1或2所述的织物涂层用阻燃聚氨酯树脂,其特征在于:所述异氰酸酯为二苯基甲烷二异氰酸酯;和/或,所述扩链剂为1,4-丁二醇、乙二醇中的一种或二者的组合;和/或,所述封端剂为甲醇;和/或,所述稳定剂为磷酸;和/或,所述溶剂为N,N-二甲基甲酰胺、甲苯中的一种或多种的组合;和/或,所述阻燃聚氨酯树脂的原料配方还包括0.01~0.1%抗氧剂。
8.一种权利要求1~7中任一项所述的织物涂层用阻燃聚氨酯树脂的制备方法,其特征在于,所述制备方法包括使聚酯多元醇、聚醚多元醇、反应型协效阻燃剂、稳定剂和一部分异氰酸酯在75±3℃下进行反应,然后降温至60~65℃,加入反应型阻燃剂进行反应,然后加入一部分溶剂和扩链剂降温,待温度降至55℃以下,加入剩余部分异氰酸酯,升温至70±5℃进行反应,反应至粘度60~80Pa.S/25℃,加入封端剂和剩余部分溶剂进行封端,制得所述阻燃聚氨酯树脂。
9.根据权利要求8所述的织物涂层用阻燃聚氨酯树脂的制备方法,其特征在于:所述反应型阻燃剂的加入按多次分批加入体系进行反应;和/或,所述一部分异氰酸酯按NCO:OH的摩尔比为1.8~2.2进行投料;和/或,所述一部分溶剂占所述溶剂总质量的50~55%进行投料。
10.根据权利要求8所述的织物涂层用阻燃聚氨酯树脂的制备方法,其特征在于:所述在75±3℃下进行反应1~3h;和/或,所述加入反应型阻燃剂份分2~4次加入体系,相邻两次间隔20~40min,所述反应型阻燃剂加入完毕,保持60~65℃反应0.5~1.5h;和/或,所述加入封端剂和剩余部分溶剂后反应5~7h。
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