CN106675375B - 一种含有有机硅改性聚氨酯丙烯酸酯的uv涂料及其制备方法和应用 - Google Patents

一种含有有机硅改性聚氨酯丙烯酸酯的uv涂料及其制备方法和应用 Download PDF

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CN106675375B
CN106675375B CN201610556315.3A CN201610556315A CN106675375B CN 106675375 B CN106675375 B CN 106675375B CN 201610556315 A CN201610556315 A CN 201610556315A CN 106675375 B CN106675375 B CN 106675375B
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叶有国
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Abstract

本发明公开一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,包括以下质量份数的原料组分:有机硅改性聚氨酯丙烯酸酯61~64份、蓖麻油基UV固化聚氨酯丙烯酸酯3~5份、乙酸仲丁酯5~7份、异丙醇7~9份、乙酸乙酯1~2份、聚醚改性聚硅氧烷流平剂0.5~1份、光引发剂2~4份、哑粉3~4份、乙酸正丁酯9~10份。通过聚醚改性聚硅氧烷流平剂配合由蓖麻油基UV固化聚氨酯丙烯酸酯和有机硅改性聚氨酯丙烯酸酯组成的混合溶液反应而成的涂料,其流平效果好、固化速度快、耐水解、耐低温,还具有电绝缘性和良好的附着力,几乎不排放挥发性有机物质,是一种综合性能优良的涂料。

Description

一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料及其制备方法 和应用
技术领域
本发明涉及一种UV涂料,特别是涉及一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料及其制备方法和应用。
背景技术
涂料因其用途广泛,对其性能要求也是因不同的用途而有所区别,有的要求具有高附着力、有的要求具有耐低温或高温性能、有的要求具有优越的电绝缘性、有的要求具有良好的耐水解性、有的要求具有抗菌性、有的要求具有较好的流平性、有的要求绿色环保等等,而大多时候,需要涂料同时具备多种优良性能,而不是单一性能,但目前市面上使用的涂料绝大多数还是性能比较单一的,这就需要开发一种能同时拥有多种优良性能的全新涂料。
发明内容
本发明的目的是克服现有技术中的不足之处,本发明的首要目的在于提供一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,该涂料不仅流平效果好、固化速度快、耐水解、耐低温,还具有电绝缘性和良好的附着力,挥发性有机物质排放量极少,是一种综合性能优良的涂料。
实现该目的的技术方案来实现的:
一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,其特征在于,由包括以下质量份数的原料组分制备而成:
更进一步的,所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料由包括以下质量份数的原料组分制备而成:
进一步的,所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料所用的蓖麻油基UV固化聚氨酯丙烯酸酯由包括以下摩尔份数的原料组分制备而成:
更进一步的,所述蓖麻油基UV固化聚氨酯丙烯酸酯由包括以下摩尔份数的原料组分制备而成:
进一步的,所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料所用的有机硅改性聚氨酯丙烯酸酯由包括以下质量份数的原料组分制备而成:
更进一步的,所述有机硅改性聚氨酯丙烯酸酯由包括以下质量份数的原料组分制备而成:
进一步的,所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料所用的聚醚改性聚硅氧烷流平剂由包括以下质量份数的原料组分制备而成:
更进一步的,所述聚醚改性聚硅氧烷流平剂由包括以下质量份数的原料组分制备而成:
本发明的目的还在于提供上述含有蓖麻油基的抗菌UV涂料的制备方法。
上述含有有机硅改性聚氨酯丙烯酸酯的UV涂料的制备方法包括如下步骤:
S1、制备蓖麻油基UV固化聚氨酯丙烯酸酯:
S11、将5.5~5.8摩尔份数的聚乙二醇、1.5~2摩尔份数的聚酯二醇和1摩尔份数的蓖麻油混合搅拌均匀并升温至110~115℃,减压脱水2.5~3h后降温至72~75℃,再分别加入1摩尔份数的异氟尔酮二异氰酸酯和0.002摩尔份数的月桂酸铋催化剂,控制滴加速度在1.5h内滴完,反应2.5~3h,得到混合溶液M;
S12、将0.3摩尔份数的N,N-二甲基甲酰胺溶于2~3摩尔份数的双酚A溶剂和0.3摩尔份数的2,2-二羟甲基丙酸溶剂中再与2~3摩尔份数的丁酮混合均匀,得到混合溶液N;
S13、将通过S12步骤配置好的混合溶液N加入S11步骤配置好的混合溶液M中,继续反应,当异氰酸基团含量达到8~13%时降温至60℃,搅拌下逐滴加 入2.2~2.5摩尔份数的丙烯酸羟乙酯和0.2摩尔份数的对苯二胺阻聚剂的混合溶液,在8min内加完,继续反应3h后监测异氰酸基团含量,当游离的异氰酸基团含量低于0.1%时,停止反应蒸出溶剂既得所述蓖麻油基UV固化聚氨酯丙烯酸酯;
S2、制备有机硅改性聚氨酯丙烯酸酯:
S21、将16~22质量份的烷羟基硅油和13~16质量份的丙烯酸-β-羟乙酯混合均匀,得到混合溶液P;
S22、将30~34质量份的异氟尔酮二异氰酸酯溶于4~6质量份的异丁醇溶剂中,加热至86~90℃,在通氮气的条件下逐滴加入通过S21配制好的混合溶液P,于2.5h滴完,恒温反应1.5h后升温到83~86℃,然后再加入4~6质量份的异丁醇溶剂和2~4质量份的过氧化苯甲酸叔丁酯引发剂,再恒温反应2.5h,待转化率达到99%后停止反应,在加热条件下减压抽滤出异丁醇溶剂,在搅拌条件下加入8~11质量份的水和4~7质量份的三乙醇胺,既得所述有机硅改性聚氨酯丙烯酸酯;
S3、制备聚醚改性聚硅氧烷流平剂:
S31、将28~33质量份的烯丙基聚醚溶于31~35质量份的乙醚溶剂中,并加入2~3质量份的氯铂酸催化剂,得到混合溶液Q;
S32、将1~2质量份的氯铂酸催化剂加入32~37质量份的含氢硅油中,在通氮气的条件下搅拌,并升温至110~115℃时逐滴加入通过S31配制好的混合溶液Q,1.5h滴完,然后在110~115℃下恒温反应4.5~5h,冷却过滤既得所述聚醚改性聚硅氧烷流平剂;
S4、制备含有有机硅改性聚氨酯丙烯酸酯的UV涂料:
S41、依次加入61~64质量份的通过S2制备而成的有机硅改性聚氨酯丙烯酸酯、3~5质量份的通过S1制备而成的蓖麻油基UV固化聚氨酯丙烯酸酯、5~7质量份的乙酸仲丁酯稀释剂、7~9质量份的异丙醇稀释剂和1~2质量份的乙酸乙酯溶剂,在800~1000r/min下分散10min;
S42、然后加入0.5~1质量份的通过S3制备而成的聚醚改性聚硅氧烷流平剂和2~4质量份的光引发剂,在600~800r/min下分散10min;
S43、在400~500r/min下缓慢加入0.95~1质量份的哑粉,然后在800~1000r/min下分散30min;
S44、最后加入9~10质量份的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至20-22s,既得所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料。
本发明还提供上述含有有机硅改性聚氨酯丙烯酸酯的UV涂料的应用。
具体的,上述含有有机硅改性聚氨酯丙烯酸酯的UV涂料的使用方法为:
用乙酸乙酯在岩田2#杯,25℃的条件下将所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料稀释到粘度为9s后喷涂在塑胶素材上,控制膜厚在15~25μm,在45~50℃下烘烤3-5min,然后用能量为800-900mj/c㎡的紫外光照射固化成膜。
与现有技术相比,本发明的优点在于:
1、蓖麻油是一种天然的可再生资源,用它代替传统的石化资源可以缓解日趋紧张的全球性石化资源危机问题,而且蓖麻油的使用不会给环境造成污染,不会给企业造成环保治理的成本压力;
2、采用双酚A溶剂和异氟尔酮二异氰酸酯同时配合蓖麻油合成蓖麻油基UV固化聚氨酯丙烯酸酯,合成的蓖麻油基UV固化聚氨酯丙烯酸酯不仅具有优良的耐水解性、耐低温、固化速度快而且其电绝缘性和附着力更是优越;
3、采用异氟尔酮二异氰酸酯、烷羟基硅油和丙烯酸-β-羟乙酯作为主要原料在异丁醇溶剂下合成的有机硅改性聚氨酯丙烯酸酯属于水性材料,对环境污染小,几乎不产生对人体有害的挥发性物质,其他溶剂则达不到如此优良效果,其与184光引发剂的配合杜绝了其本身固化时间长的缺点;
4、采用乙醚作为溶剂,将含氢硅油和烯丙基聚醚在氯铂酸催化剂的催化下合成的聚醚改性聚硅氧烷流平剂具有良好的低表面张力和相容性,其表面状态控制能力优越,其它溶剂和催化剂的配合得到的聚醚改性聚硅氧烷流平剂却不能达到如此效果;
5、通过聚醚改性聚硅氧烷流平剂配合由蓖麻油基UV固化聚氨酯丙烯酸酯和有机硅改性聚氨酯丙烯酸酯按一定比例配比而成的混合溶液聚合出的涂料,其流平效果好、挥发性有机物质排放少,还具有耐水解性、耐低温,而且其电 绝缘性和附着力更是优越,是一种综合性能优良的涂料。
具体实施方式
下面结合实施例对本发明作进一步详细的描述,但本发明的实施方式不限于此。
实施例1
传统光固化涂料的制备方法:
①依次加入51g的聚氨酯丙烯酸酯、7g的乙酸仲丁酯稀释剂、7g的异丙醇稀释剂和1g的乙酸乙酯溶剂,在800r/min下分散10min;
②然后加入0.5g的丙烯酸树脂流平剂和2g的184光引发剂,在800r/min下分散10min;
③在500r/min下缓慢加入3g的哑粉,然后在800r/min下分散30min;
④最后加入9g的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至20s,既得传统光固化涂料。
实施例2
一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,其由以下组分配比及制备方法制备而成:
S1、制备蓖麻油基UV固化聚氨酯丙烯酸酯:
S11、将5.8mol的聚乙二醇、1.5mol的聚酯二醇和1mol的蓖麻油混合搅拌均匀并升温至115℃,减压脱水2.5h后降温至75℃,再分别加入1mol的异氟尔酮二异氰酸酯和0.002mol的月桂酸铋催化剂,控制滴加速度在1.5h内滴完,反应3h,得到混合溶液M;
S12、将0.3mol的N,N-二甲基甲酰胺溶于2mol的双酚A溶剂和0.3mol的2,2-二羟甲基丙酸溶剂中再与3mol的丁酮混合均匀,得到混合溶液N;
S13、将通过S12步骤配置好的混合溶液N加入S11步骤配置好的混合溶液 M中,继续反应,当异氰酸基团含量达到8%时降温至60℃,搅拌下逐滴加入2.5mol的丙烯酸羟乙酯和0.2mol的对苯二胺阻聚剂的混合溶液,在8min内加完,继续反应3h后监测异氰酸基团含量,当游离的异氰酸基团含量低于0.1%时,停止反应蒸出溶剂既得所述蓖麻油基UV固化聚氨酯丙烯酸酯;
S2、制备有机硅改性聚氨酯丙烯酸酯:
S21、将16g的烷羟基硅油和13g的丙烯酸-β-羟乙酯混合均匀,得到混合溶液P;
S22、将34g的异氟尔酮二异氰酸酯溶于6g的异丁醇溶剂中,加热至86℃,在通氮气的条件下逐滴加入通过S21配制好的混合溶液P,于2.5h滴完,恒温反应1.5h后升温到86℃,然后再加入6g的异丁醇溶剂和4g的过氧化苯甲酸叔丁酯引发剂,再恒温反应2.5h,待转化率达到99%后停止反应,在加热条件下减压抽滤出异丁醇溶剂,在搅拌条件下加入8g的水和4g的三乙醇胺,既得所述有机硅改性聚氨酯丙烯酸酯;
S3、制备聚醚改性聚硅氧烷流平剂:
S31、将33g的烯丙基聚醚溶于35g的乙醚溶剂中,并加入3g的氯铂酸催化剂,得到混合溶液Q;
S32、将1g的氯铂酸催化剂加入32g的含氢硅油中,在通氮气的条件下搅拌,并升温至110℃时逐滴加入通过S31配制好的混合溶液Q,1.5h滴完,然后在110℃下恒温反应4.5h,冷却过滤既得所述聚醚改性聚硅氧烷流平剂;
S4、制备含有有机硅改性聚氨酯丙烯酸酯的UV涂料:
S41、依次加入61g的通过S2制备而成的有机硅改性聚氨酯丙烯酸酯、5g的通过S1制备而成的蓖麻油基UV固化聚氨酯丙烯酸酯、5g的乙酸仲丁酯稀释剂、9g的异丙醇稀释剂和2g的乙酸乙酯溶剂,在800r/min下分散10min;
S42、然后加入1g的通过S3制备而成的聚醚改性聚硅氧烷流平剂和4g的184光引发剂,在800r/min下分散10min;
S43、在500r/min下缓慢加入4g的哑粉,然后在800r/min下分散30min;
S44、最后加入9g的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至20s,既得所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料。
实施例3
一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,其由以下组分配比及制备方法制备而成:
S1、制备蓖麻油基UV固化聚氨酯丙烯酸酯:
S11、将5.5mol的聚乙二醇、2mol的聚酯二醇和1mol的蓖麻油混合搅拌均匀并升温至110℃,减压脱水3h后降温至72℃,再分别加入1mol的异氟尔酮二异氰酸酯和0.002mol的月桂酸铋催化剂,控制滴加速度在1.5h内滴完,反应2.5h,得到混合溶液M;
S12、将0.3mol的N,N-二甲基甲酰胺溶于3mol的双酚A溶剂和0.3mol的2,2-二羟甲基丙酸溶剂中再与2mol的丁酮混合均匀,得到混合溶液N;
S13、将通过S12步骤配置好的混合溶液N加入S11步骤配置好的混合溶液M中,继续反应,当异氰酸基团含量达到13%时降温至60℃,搅拌下逐滴加入2.2mol的丙烯酸羟乙酯和0.2mol的对苯二胺阻聚剂的混合溶液,在8min内加完,继续反应3h后监测异氰酸基团含量,当游离的异氰酸基团含量低于0.1%时,停止反应蒸出溶剂既得所述蓖麻油基UV固化聚氨酯丙烯酸酯;
S2、制备有机硅改性聚氨酯丙烯酸酯:
S21、将22g的烷羟基硅油和16g的丙烯酸-β-羟乙酯混合均匀,得到混合溶液P;
S22、将30g的异氟尔酮二异氰酸酯溶于4g的异丁醇溶剂中,加热至90℃,在通氮气的条件下逐滴加入通过S21配制好的混合溶液P,于2.5h滴完,恒温反应1.5h后升温到83℃,然后再加入4g的异丁醇溶剂和2g的过氧化苯甲酸叔丁酯引发剂,再恒温反应2.5h,待转化率达到99%后停止反应,在加热条件下减压抽滤出异丁醇溶剂,在搅拌条件下加入11g的水和7g的三乙醇胺,既得所述有机硅改性聚氨酯丙烯酸酯;
S3、制备聚醚改性聚硅氧烷流平剂:
S31、将28g的烯丙基聚醚溶于31g的乙醚溶剂中,并加入2g的氯铂酸催化剂,得到混合溶液Q;
S32、将2g的氯铂酸催化剂加入37g的含氢硅油中,在通氮气的条件下搅 拌,并升温至115℃时逐滴加入通过S31配制好的混合溶液Q,1.5h滴完,然后在115℃下恒温反应5h,冷却过滤既得所述聚醚改性聚硅氧烷流平剂;
S4、制备含有有机硅改性聚氨酯丙烯酸酯的UV涂料:
S41、依次加入64g的通过S2制备而成的有机硅改性聚氨酯丙烯酸酯、3g的通过S1制备而成的蓖麻油基UV固化聚氨酯丙烯酸酯、4g的乙酸仲丁酯稀释剂、7g的异丙醇稀释剂和1g的乙酸乙酯溶剂,在1000r/min下分散10min;
S42、然后加入0.5g的通过S3制备而成的聚醚改性聚硅氧烷流平剂和2g的184光引发剂,在600r/min下分散10min;
S43、在400r/min下缓慢加入3g的哑粉,然后在1000r/min下分散30min;
S44、最后加入10g的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至22s,既得所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料。
实施例4
一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料,其由以下组分配比及制备方法制备而成:
S1、制备蓖麻油基UV固化聚氨酯丙烯酸酯:
S11、将5.8mol的聚乙二醇、1.5mol的聚酯二醇和1mol的蓖麻油混合搅拌均匀并升温至115℃,减压脱水3h后降温至75℃,再分别加入1Mol的异氟尔酮二异氰酸酯和0.002mol的月桂酸铋催化剂,控制滴加速度在1.5h内滴完,反应3h,得到混合溶液M;
S12、将0.3mol的N,N-二甲基甲酰胺溶于2mol的双酚A溶剂和0.3mol的2,2-二羟甲基丙酸溶剂中再与2mol的丁酮混合均匀,得到混合溶液N;
S13、将通过S12步骤配置好的混合溶液N加入S11步骤配置好的混合溶液M中,继续反应,当异氰酸基团含量达到13%时降温至60℃,搅拌下逐滴加入2.5mol的丙烯酸羟乙酯和0.2mol的对苯二胺阻聚剂的混合溶液,在8min内加完,继续反应3h后监测异氰酸基团含量,当游离的异氰酸基团含量低于0.1%时,停止反应蒸出溶剂既得所述蓖麻油基UV固化聚氨酯丙烯酸酯;
S2、制备有机硅改性聚氨酯丙烯酸酯:
S21、将19g的烷羟基硅油和16g的丙烯酸-β-羟乙酯混合均匀,得到混合 溶液P;
S22、将33g的异氟尔酮二异氰酸酯溶于6g的异丁醇溶剂中,加热至90℃,在通氮气的条件下逐滴加入通过S21配制好的混合溶液P,于2.5h滴完,恒温反应1.5h后升温到86℃,然后再加入6g的异丁醇溶剂和4g的过氧化苯甲酸叔丁酯引发剂,再恒温反应2.5h,待转化率达到99%后停止反应,在加热条件下减压抽滤出异丁醇溶剂,在搅拌条件下加入10g的水和6g的三乙醇胺,既得所述有机硅改性聚氨酯丙烯酸酯;
S3、制备聚醚改性聚硅氧烷流平剂:
S31、将30g的烯丙基聚醚溶于33g的乙醚溶剂中,并加入3g的氯铂酸催化剂,得到混合溶液Q;
S32、将2g的氯铂酸催化剂加入32g的含氢硅油中,在通氮气的条件下搅拌,并升温至115℃时逐滴加入通过S31配制好的混合溶液Q,1.5h滴完,然后在115℃下恒温反应5h,冷却过滤既得所述聚醚改性聚硅氧烷流平剂;
S4、制备含有有机硅改性聚氨酯丙烯酸酯的UV涂料:
S41、依次加入63g的通过S2制备而成的有机硅改性聚氨酯丙烯酸酯、5g的通过S1制备而成的蓖麻油基UV固化聚氨酯丙烯酸酯、6g的乙酸仲丁酯稀释剂、8g的异丙醇稀释剂和2g的乙酸乙酯溶剂,在1000r/min下分散10min;
S42、然后加入0.5g的通过S3制备而成的聚醚改性聚硅氧烷流平剂和3g的184光引发剂,在800r/min下分散10min;
S43、在400r/min下缓慢加入3.3g的哑粉,然后在800r/min下分散30min;
S44、最后加入9.2g的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至22s,既得所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料。
所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料的使用方法为:
用乙酸乙酯在岩田2#杯,25℃的条件下将所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料稀释到粘度为9s后喷涂在塑胶素材上,控制膜厚在15~25μm,在45~50℃下烘烤3-5min,然后用能量为800-900mj/c㎡的紫外光照射固化成膜。
通过常规测试方法分别对实施例1至4制备出的涂料进行测试,测试结果 见下表:
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。

Claims (1)

1.一种含有有机硅改性聚氨酯丙烯酸酯的UV涂料的制备方法为:
S1、制备蓖麻油基UV固化聚氨酯丙烯酸酯:
S11、将5.5~5.8摩尔份数的聚乙二醇、1.5~2摩尔份数的聚酯二醇和1摩尔份数的蓖麻油混合搅拌均匀并升温至110~115℃,减压脱水2.5~3h后降温至72~75℃,再分别加入1摩尔份数的异氟尔酮二异氰酸酯和0.002摩尔份数的月桂酸铋催化剂,控制滴加速度在1.5h内滴完,反应2.5~3h,得到混合溶液M;
S12、将0.3摩尔份数的N,N-二甲基甲酰胺溶于2~3摩尔份数的双酚A溶剂和0.3摩尔份数的2,2-二羟甲基丙酸溶剂中再与2~3摩尔份数的丁酮混合均匀,得到混合溶液N;
S13、将通过S12步骤配置好的混合溶液N加入S11步骤配置好的混合溶液M中,继续反应,当异氰酸基团含量达到8~13%时降温至60℃,搅拌下逐滴加入2.2~2.5摩尔份数的丙烯酸羟乙酯和0.2摩尔份数的对苯二胺阻聚剂的混合溶液,在8min内加完,继续反应3h后监测异氰酸基团含量,当游离的异氰酸基团含量低于0.1%时,停止反应蒸出溶剂既得所述蓖麻油基UV固化聚氨酯丙烯酸酯;
S2、制备有机硅改性聚氨酯丙烯酸酯:
S21、将16~22质量份的烷羟基硅油和13~16质量份的丙烯酸-β-羟乙酯混合均匀,得到混合溶液P;
S22、将30~34质量份的异氟尔酮二异氰酸酯溶于4~6质量份的异丁醇溶剂中,加热至86~90℃,在通氮气的条件下逐滴加入通过S21配制好的混合溶液P,于2.5h滴完,恒温反应1.5h后升温到83~86℃,然后再加入4~6质量份的异丁醇溶剂和2~4质量份的过氧化苯甲酸叔丁酯引发剂,再恒温反应2.5h,待转化率达到99%后停止反应,在加热条件下减压抽滤出异丁醇溶剂,在搅拌条件下加入8~11质量份的水和4~7质量份的三乙醇胺,既得所述有机硅改性聚氨酯丙烯酸酯;
S3、制备聚醚改性聚硅氧烷流平剂:
S31、将28~33质量份的烯丙基聚醚溶于31~35质量份的乙醚溶剂中,并加入2~3质量份的氯铂酸催化剂,得到混合溶液Q;
S32、将1~2质量份的氯铂酸催化剂加入32~37质量份的含氢硅油中,在通氮气的条件下搅拌,并升温至110~115℃时逐滴加入通过S31配制好的混合溶液Q,1.5h滴完,然后在110~115℃下恒温反应4.5~5h,冷却过滤既得所述聚醚改性聚硅氧烷流平剂;
S4、制备含有有机硅改性聚氨酯丙烯酸酯的UV涂料:
S41、依次加入61~64质量份的通过S2制备而成的有机硅改性聚氨酯丙烯酸酯、3~5质量份的通过S1制备而成的蓖麻油基UV固化聚氨酯丙烯酸酯、5~7质量份的乙酸仲丁酯稀释剂、7~9质量份的异丙醇稀释剂和1~2质量份的乙酸乙酯溶剂,在800~1000r/min下分散10min;
S42、然后加入0.5~1质量份的通过S3制备而成的聚醚改性聚硅氧烷流平剂和2~4质量份的光引发剂,在600~800r/min下分散10min;
S43、在400~500r/min下缓慢加入0.95~1质量份的哑粉,然后在800~1000r/min下分散30min;
S44、最后加入9~10质量份的乙酸正丁酯溶剂在岩田2#杯,25℃的条件下调整粘度至20-22s,既得所述含有有机硅改性聚氨酯丙烯酸酯的UV涂料。
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CN108411695A (zh) * 2018-02-05 2018-08-17 东莞嘉颐实业有限公司 一种免打底uv光油及其制备方法和应用
CN109627738B (zh) * 2018-12-06 2021-04-02 马东晖 一种有机硅改性Ms路面墙面建筑材料及制造工艺
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102229779A (zh) * 2011-06-20 2011-11-02 上虞市佑谦特种材料有限公司 Uv消光漆及其制备方法
CN102643565A (zh) * 2012-05-04 2012-08-22 浙江润禾有机硅新材料有限公司 一种终端改性有机硅涂料流平剂及其制备方法
CN103555192A (zh) * 2013-11-21 2014-02-05 武汉大学 一种有机硅改性的水性uv涂料及其制备方法
CN104387945A (zh) * 2014-10-24 2015-03-04 崇州市美涂士涂料科技有限公司 一种净味耐污耐黄变uv覆膜哑光面漆涂料及其制备方法与施工工艺

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102229779A (zh) * 2011-06-20 2011-11-02 上虞市佑谦特种材料有限公司 Uv消光漆及其制备方法
CN102643565A (zh) * 2012-05-04 2012-08-22 浙江润禾有机硅新材料有限公司 一种终端改性有机硅涂料流平剂及其制备方法
CN103555192A (zh) * 2013-11-21 2014-02-05 武汉大学 一种有机硅改性的水性uv涂料及其制备方法
CN104387945A (zh) * 2014-10-24 2015-03-04 崇州市美涂士涂料科技有限公司 一种净味耐污耐黄变uv覆膜哑光面漆涂料及其制备方法与施工工艺

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《蓖麻油基UV固化聚氨酯丙烯酸酯的合成及固化膜性能》;黄家健等;《高分子材料科学与工程》;20160430;第32卷(第4期);第23页左栏第一段,第24页1.2实验原理与步骤,第29页3结论

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