CN108359325A - 一种用于机械设备的防火涂料的制备方法 - Google Patents
一种用于机械设备的防火涂料的制备方法 Download PDFInfo
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Abstract
本发明提供一种用于机械设备的防火涂料的制备方法,包括以下步骤:a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合搅拌,再加入阻燃复合液,超声分散,得到材料一;b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨,再加入到改性醋酸乙烯酯‑叔碳酸乙烯酯乳液中,加入环氧树脂和有机硅树脂,加热搅拌至熔融状态,保温得到材料二;c、向材料二中加入改性硼酚醛树脂和加工助剂,搅拌得到材料三;d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,研磨分散后,脱水处理。本发明制备的防火涂料物理、机械性能稳定,抗开裂性能及耐水性能优秀,耐火性能优异。
Description
技术领域
本发明属于防火涂料技术领域,具体涉及一种用于机械设备的防火涂料的制备方法。
背景技术
目前,防火涂料在石油化工(如炼油厂、石油钻井平台、储油罐支撑等)、电力、工业及民用建筑(如工业厂房、大型体育馆钢结构)、机械等行业应用也越来越广,所以,即耐候防腐又高效阻燃的防火涂料研制迫在眉捷。
防火涂料涂覆于物体表面,在遇火时涂膜本身难燃或不燃,对基材有较好的保护作用,为灭火和人员撤离赢得了时间。因此对它的研究和应用已引起了世界各国的高度重视。防火涂料依其防火机理不同可分为非膨胀型与膨胀型两类,其中非膨胀型防火涂料在燃烧中吸收大量的热量,使温度难以上升,其自身不燃烧并形成一层隔绝氧气的釉状保护层,对物体起到一定的保护作用,但隔热性能较差。而膨胀型防火涂料平常保持普通涂膜状态,遇火时,涂层发生软化熔融,膨胀形成海绵状或蜂窝状炭化层,虽然其防火性能较好,但是其以甲醛作为其炭化剂,会在使用时散发出有毒气体,给人的身体健康带来危害。
综上所述,因此需要一种更好的防火涂料,来改善现有技术的不足。
发明内容
本发明的目的是提供一种用于机械设备的防火涂料的制备方法,本发明制备的防火涂料保护期限长、防火效果好,且机械性能、耐候性和防腐性佳,无毒、环保、应用泛围广。
本发明提供了如下的技术方案:
一种用于机械设备的防火涂料的制备方法,包括以下制备步骤:
a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合导入混料机中,机械搅拌混合30-40min,再加入阻燃复合液,超声分散20-25min,得到材料一;
b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨1-2h,再加入到改性醋酸乙烯酯-叔碳酸乙烯酯乳液中,再加入环氧树脂和有机硅树脂,在280-350℃下加热搅拌至熔融状态,保温1-2h,得到材料二;
c、向材料二中加入改性硼酚醛树脂和加工助剂,在200-300r/min的转速下搅拌40-50min,得到材料三;
d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,在高速研磨分散机中,以1600-1800r/min的转速研磨分散15-25min,研磨分散后出料,再置于80-90℃下脱水处理10-15min,即可得到成品。
优选的,所述步骤a的改性石墨的制备方法为:将石墨水洗、除尘、筛分去除杂质,经80-120℃烘干后,用硫酸和冰醋酸配制成的混合酸化液酸化处理,在40-45℃水浴温度下,搅拌反应30-40min,然后加入强氧化剂并搅拌15-20min,经抽滤脱酸、水洗至PH值为6-7、脱水干燥,在600-800℃下,膨胀形成改性石墨。
优选的,所述步骤a的阻燃复合液的制备方法为:将纳米二氧化钛和纳米镁铝水滑石加入丙酮溶液中,经30-45min的分散处理,再加入流平剂、消烟剂,超声分散1-2h,即可得到阻燃复合液。
优选的,所述步骤b的无机填料为绢云母和滑石粉的混合物。
优选的,所述步骤b的改性醋酸乙烯酯-叔碳酸乙烯酯乳液的制备方法为:将醋酸乙烯酯-叔碳酸乙烯酯乳液加入到反应釜中,升温至45-55℃,在200-240r/min的搅拌速度下搅拌20-25min,搅拌过程中滴加3-(2,3-环氧丙氧)丙基三甲氧基硅烷,滴加完毕后,再保温反应1-2h,降至常温后,即可得到改性醋酸乙烯酯-叔碳酸乙烯酯乳液。
优选的,所述步骤c的改性硼酚醛树脂的制备方法为:将聚合松香加热至完全融化,向融化的聚合松香中加入硼酚醛树脂、氧化铁、过硫酸钾和马来酸酐,在220-240℃下搅拌反应25-40min,再降温至90-110℃,搅拌反应1-2h,反应结束后冷却至室温,即可得到改性硼酚醛树脂。
优选的,所述步骤c的加工助剂的制备方法为:将聚磷酸铵、季戊四醇、三聚氰胺、钛白粉和氯化石蜡依次加入分散罐中,在1200-1500r/min的转速分散30-35min,再研磨20-30min后过滤,加入聚氧丙烯甘油醚消泡剂,消泡30-40min,即可得到加工助剂。
优选的,所述步骤d的成膜助剂为醇酯-12、二丙二醇丁醚和二丙二醇甲醚中的任一种或几种的混合。
本发明的有益效果是:
本发明制备的防火涂料抗压强度高,不易脱落、起泡,防火涂料保护期限长、防火效果好,且机械性能、耐候性和防腐性佳,无毒、环保、应用泛围广,其制备步骤简单,所需成本低,同时不含有害物质,不会危害人的身体健康。
本发明中的阻燃复合液中纳米粒子可大大提高其与基料的相容性和防火阻燃性,而且可提高涂料的机械性能、耐候性和防腐性。
本发明制备的防火涂料具有很好的防火隔热性能,附着力好,且强度高。它能承受高低温循环的影响,耐盐雾、耐工业大气腐蚀、 耐酸、碱、盐腐蚀,且具有不易脱落,贮存稳定,施工方便的优点。
具体实施方式
实施例1
一种用于机械设备的防火涂料的制备方法,包括以下制备步骤:
a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合导入混料机中,机械搅拌混合40min,再加入阻燃复合液,超声分散20min,得到材料一;
b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨1h,再加入到改性醋酸乙烯酯-叔碳酸乙烯酯乳液中,再加入环氧树脂和有机硅树脂,在350℃下加热搅拌至熔融状态,保温2h,得到材料二;
c、向材料二中加入改性硼酚醛树脂和加工助剂,在200r/min的转速下搅拌50min,得到材料三;
d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,在高速研磨分散机中,以1800r/min的转速研磨分散15min,研磨分散后出料,再置于80℃下脱水处理15min,即可得到成品。
步骤a的改性石墨的制备方法为:将石墨水洗、除尘、筛分去除杂质,经80℃烘干后,用硫酸和冰醋酸配制成的混合酸化液酸化处理,在45℃水浴温度下,搅拌反应30min,然后加入强氧化剂并搅拌20min,经抽滤脱酸、水洗至PH值为6、脱水干燥,在800℃下,膨胀形成改性石墨。
步骤a的阻燃复合液的制备方法为:将纳米二氧化钛和纳米镁铝水滑石加入丙酮溶液中,经30min的分散处理,再加入流平剂、消烟剂,超声分散2h,即可得到阻燃复合液。
步骤b的无机填料为绢云母和滑石粉的混合物。
步骤b的改性醋酸乙烯酯-叔碳酸乙烯酯乳液的制备方法为:将醋酸乙烯酯-叔碳酸乙烯酯乳液加入到反应釜中,升温至55℃,在200r/min的搅拌速度下搅拌20min,搅拌过程中滴加3-(2,3-环氧丙氧)丙基三甲氧基硅烷,滴加完毕后,再保温反应2h,降至常温后,即可得到改性醋酸乙烯酯-叔碳酸乙烯酯乳液。
步骤c的改性硼酚醛树脂的制备方法为:将聚合松香加热至完全融化,向融化的聚合松香中加入硼酚醛树脂、氧化铁、过硫酸钾和马来酸酐,在220℃下搅拌反应40min,再降温至110℃,搅拌反应1h,反应结束后冷却至室温,即可得到改性硼酚醛树脂。
步骤c的加工助剂的制备方法为:将聚磷酸铵、季戊四醇、三聚氰胺、钛白粉和氯化石蜡依次加入分散罐中,在1200r/min的转速分散30min,再研磨30min后过滤,加入聚氧丙烯甘油醚消泡剂,消泡40min,即可得到加工助剂。
步骤d的成膜助剂为醇酯-12、二丙二醇丁醚和二丙二醇甲醚的混合。
实施例2
一种用于机械设备的防火涂料的制备方法,包括以下制备步骤:
a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合导入混料机中,机械搅拌混合30min,再加入阻燃复合液,超声分散25min,得到材料一;
b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨1h,再加入到改性醋酸乙烯酯-叔碳酸乙烯酯乳液中,再加入环氧树脂和有机硅树脂,在280℃下加热搅拌至熔融状态,保温1h,得到材料二;
c、向材料二中加入改性硼酚醛树脂和加工助剂,在200r/min的转速下搅拌40min,得到材料三;
d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,在高速研磨分散机中,以1600r/min的转速研磨分散15min,研磨分散后出料,再置于80℃下脱水处理10min,即可得到成品。
步骤a的改性石墨的制备方法为:将石墨水洗、除尘、筛分去除杂质,经80℃烘干后,用硫酸和冰醋酸配制成的混合酸化液酸化处理,在40℃水浴温度下,搅拌反应30min,然后加入强氧化剂并搅拌15min,经抽滤脱酸、水洗至PH值为6、脱水干燥,在600℃下,膨胀形成改性石墨。
步骤a的阻燃复合液的制备方法为:将纳米二氧化钛和纳米镁铝水滑石加入丙酮溶液中,经30min的分散处理,再加入流平剂、消烟剂,超声分散1h,即可得到阻燃复合液。
步骤b的无机填料为绢云母和滑石粉的混合物。
步骤b的改性醋酸乙烯酯-叔碳酸乙烯酯乳液的制备方法为:将醋酸乙烯酯-叔碳酸乙烯酯乳液加入到反应釜中,升温至45℃,在200r/min的搅拌速度下搅拌20min,搅拌过程中滴加3-(2,3-环氧丙氧)丙基三甲氧基硅烷,滴加完毕后,再保温反应1h,降至常温后,即可得到改性醋酸乙烯酯-叔碳酸乙烯酯乳液。
步骤c的改性硼酚醛树脂的制备方法为:将聚合松香加热至完全融化,向融化的聚合松香中加入硼酚醛树脂、氧化铁、过硫酸钾和马来酸酐,在220℃下搅拌反应25min,再降温至90℃,搅拌反应1h,反应结束后冷却至室温,即可得到改性硼酚醛树脂。
步骤c的加工助剂的制备方法为:将聚磷酸铵、季戊四醇、三聚氰胺、钛白粉和氯化石蜡依次加入分散罐中,在1200r/min的转速分散30min,再研磨20min后过滤,加入聚氧丙烯甘油醚消泡剂,消泡30min,即可得到加工助剂。
步骤d的成膜助剂为醇酯-12、二丙二醇丁醚和二丙二醇甲醚的混合。
实施例3
一种用于机械设备的防火涂料的制备方法,包括以下制备步骤:
a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合导入混料机中,机械搅拌混合40min,再加入阻燃复合液,超声分散25min,得到材料一;
b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨2h,再加入到改性醋酸乙烯酯-叔碳酸乙烯酯乳液中,再加入环氧树脂和有机硅树脂,在350℃下加热搅拌至熔融状态,保温2h,得到材料二;
c、向材料二中加入改性硼酚醛树脂和加工助剂,在300r/min的转速下搅拌50min,得到材料三;
d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,在高速研磨分散机中,以1600/min的转速研磨分散25min,研磨分散后出料,再置于90℃下脱水处理15min,即可得到成品。
步骤a的改性石墨的制备方法为:将石墨水洗、除尘、筛分去除杂质,经120℃烘干后,用硫酸和冰醋酸配制成的混合酸化液酸化处理,在45℃水浴温度下,搅拌反应40min,然后加入强氧化剂并搅拌20min,经抽滤脱酸、水洗至PH值为7、脱水干燥,在800℃下,膨胀形成改性石墨。
步骤a的阻燃复合液的制备方法为:将纳米二氧化钛和纳米镁铝水滑石加入丙酮溶液中,经45min的分散处理,再加入流平剂、消烟剂,超声分散2h,即可得到阻燃复合液。
步骤b的无机填料为绢云母和滑石粉的混合物。
步骤b的改性醋酸乙烯酯-叔碳酸乙烯酯乳液的制备方法为:将醋酸乙烯酯-叔碳酸乙烯酯乳液加入到反应釜中,升温至55℃,在240r/min的搅拌速度下搅拌25min,搅拌过程中滴加3-(2,3-环氧丙氧)丙基三甲氧基硅烷,滴加完毕后,再保温反应2h,降至常温后,即可得到改性醋酸乙烯酯-叔碳酸乙烯酯乳液。
步骤c的改性硼酚醛树脂的制备方法为:将聚合松香加热至完全融化,向融化的聚合松香中加入硼酚醛树脂、氧化铁、过硫酸钾和马来酸酐,在240℃下搅拌反应40min,再降温至110℃,搅拌反应2h,反应结束后冷却至室温,即可得到改性硼酚醛树脂。
步骤c的加工助剂的制备方法为:将聚磷酸铵、季戊四醇、三聚氰胺、钛白粉和氯化石蜡依次加入分散罐中,在1500r/min的转速分散35min,再研磨30min后过滤,加入聚氧丙烯甘油醚消泡剂,消泡40min,即可得到加工助剂。
步骤d的成膜助剂为醇酯-12、二丙二醇丁醚和二丙二醇甲醚的混合。
检测以上实施例制备的成品,得到以下实验数据:
表一:
项目 | 在容器中状态 | 表干时间(h) | 外观与颜色 | 耐水性 | 耐冷热循环性(次) |
实施例1 | 搅拌后呈均匀细腻状态,无结块 | ≤3 | 涂层干燥后,外观与颜色同样品相比无差别 | 浸泡48h,涂层无起泡、脱落现象 | 20次循环,无开裂、剥落、裂纹 |
实施例2 | 搅拌后呈均匀细腻状态,无结块 | ≤3 | 涂层干燥后,外观与颜色同样品相比无差别 | 浸泡48h,涂层无起泡、脱落现象 | 20次循环,无开裂、剥落、裂纹 |
实施例3 | 搅拌后呈均匀细腻状态,无结块 | ≤3 | 涂层干燥后,外观与颜色同样品相比无差别 | 浸泡48h,涂层无起泡、脱落现象 | 20次循环,无开裂、剥落、裂纹 |
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (8)
1.一种用于机械设备的防火涂料的制备方法,其特征在于,包括以下制备步骤:
a、将改性石墨、丙烯酸树脂、增强玻璃纤维和氯化石蜡混合导入混料机中,机械搅拌混合30-40min,再加入阻燃复合液,超声分散20-25min,得到材料一;
b、将无机填料、纳米二氧化硅、羧甲基纤维素和桐油混合球磨1-2h,再加入到改性醋酸乙烯酯-叔碳酸乙烯酯乳液中,再加入环氧树脂和有机硅树脂,在280-350℃下加热搅拌至熔融状态,保温1-2h,得到材料二;
c、向材料二中加入改性硼酚醛树脂和加工助剂,在200-300r/min的转速下搅拌40-50min,得到材料三;
d、将材料一、材料三混合搅拌均匀,再加入成膜助剂、表面改性剂和增稠剂,在高速研磨分散机中,以1600-1800r/min的转速研磨分散15-25min,研磨分散后出料,再置于80-90℃下脱水处理10-15min,即可得到成品。
2.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤a的改性石墨的制备方法为:将石墨水洗、除尘、筛分去除杂质,经80-120℃烘干后,用硫酸和冰醋酸配制成的混合酸化液酸化处理,在40-45℃水浴温度下,搅拌反应30-40min,然后加入强氧化剂并搅拌15-20min,经抽滤脱酸、水洗至PH值为6-7、脱水干燥,在600-800℃下,膨胀形成改性石墨。
3.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤a的阻燃复合液的制备方法为:将纳米二氧化钛和纳米镁铝水滑石加入丙酮溶液中,经30-45min的分散处理,再加入流平剂、消烟剂,超声分散1-2h,即可得到阻燃复合液。
4.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤b的无机填料为绢云母和滑石粉的混合物。
5.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤b的改性醋酸乙烯酯-叔碳酸乙烯酯乳液的制备方法为:将醋酸乙烯酯-叔碳酸乙烯酯乳液加入到反应釜中,升温至45-55℃,在200-240r/min的搅拌速度下搅拌20-25min,搅拌过程中滴加3-(2,3-环氧丙氧)丙基三甲氧基硅烷,滴加完毕后,再保温反应1-2h,降至常温后,即可得到改性醋酸乙烯酯-叔碳酸乙烯酯乳液。
6.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤c的改性硼酚醛树脂的制备方法为:将聚合松香加热至完全融化,向融化的聚合松香中加入硼酚醛树脂、氧化铁、过硫酸钾和马来酸酐,在220-240℃下搅拌反应25-40min,再降温至90-110℃,搅拌反应1-2h,反应结束后冷却至室温,即可得到改性硼酚醛树脂。
7.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤c的加工助剂的制备方法为:将聚磷酸铵、季戊四醇、三聚氰胺、钛白粉和氯化石蜡依次加入分散罐中,在1200-1500r/min的转速分散30-35min,再研磨20-30min后过滤,加入聚氧丙烯甘油醚消泡剂,消泡30-40min,即可得到加工助剂。
8.根据权利要求1所述的一种用于机械设备的防火涂料的制备方法,其特征在于,所述步骤d的成膜助剂为醇酯-12、二丙二醇丁醚和二丙二醇甲醚中的任一种或几种的混合。
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