CN106590327A - 一种含钛‑硼有机硅改性环氧树脂耐磨涂料及其制备方法 - Google Patents
一种含钛‑硼有机硅改性环氧树脂耐磨涂料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含钛‑硼有机硅改性环氧树脂耐磨涂料,及其制备工艺,其特征在于,以环氧树脂E‑20、甲基三乙氧基硅烷、二月桂酸二丁基锡、聚酰胺固化剂、硼酸、钛酸丁酯、纳米氧化锑锡、纳米TiO2、KH‑570、聚乙烯醇、高岭土、Sb2O3、聚磷酸铵、空心玻璃微珠、滑石粉、MoS2粉、SiC粉、膨润土等为原料。本发明合成了含钛‑硼有机硅树脂;KH‑570改性ATO粉体、纳米TiO2,制成稳定的分散良好的料浆;用球磨法制备了Sb2O3/高岭土复合阻燃微粉,与聚磷酸铵并用,产生协同效应,阻燃效果更佳;即得到一种含钛‑硼有机硅改性环氧树脂耐磨涂料。
Description
技术领域
本发明涉及复合材料领域,具体涉及一种含钛-硼有机硅改性环氧树脂耐磨涂料,及其制备工艺。
背景技术
有机硅树脂广泛用于耐高温防腐涂料、耐高温绝缘涂料、耐高温防火隔热阻燃涂料等,但存在附着力差、温度较高时漆膜的力学强度降低等问题,使其应用受到限制。用一些具有优良耐温性和绝缘性的无机材料对有机树脂进行改性和掺杂,是近年来一个新的研究方向。环氧树脂由于具有许多优异的性能而广泛应用于耐腐蚀涂料领域,但存在耐高温性差、韧性差、质脆等缺点,以有机硅聚合物改性环氧树脂用以提高环氧树脂涂料的韧性、耐热性、耐腐蚀性具有重要的意义。
厐玉宁在其硕士学位论文《有机硅改性环氧树脂涂料制备及性能研究》一文中,以一甲基三乙氧基硅烷、二甲基二乙氧基硅烷、苯基三乙氧基硅烷为原材料,在催化剂HCl的作用下,经过水解缩合反应后,形成有机硅聚合物;以有机硅聚合物作为改性剂,对环氧树脂E-20进行改性,以改性后的树脂作为基体,加入各种颜填料、助剂及固化剂制备得耐高温防腐涂料。但是存在耐高温防腐性能不足。
本发明以甲基三乙氧基硅烷为硅源、钛酸丁酯为钛源、硼酸为硼源、HCl为催化剂,二甲苯为溶剂,二月桂酸二丁基锡为催化剂,经水解-缩合反应合成了含钛-硼有机硅树脂;KH-570改性ATO粉体、纳米TiO2,以聚乙烯醇为分散剂,制成稳定的分散良好的料浆,用改性环氧树脂作为成膜物,制备了透明隔热涂料;用球磨法制备了Sb2O3/高岭土复合阻燃微粉,Sb2O3属于添加型阻燃剂,以锑白粉为主,高岭土附在锑白粉表面,充分与锑白粉发生物理、化学作用,与聚磷酸铵并用,产生协同效应,阻燃效果更佳;即得到一种含钛-硼有机硅改性环氧树脂耐磨涂料。
发明内容
本发明主要解决的技术问题是提供一种含钛-硼有机硅改性环氧树脂耐磨涂料及其制备工艺,依照该工艺制作的涂料耐高温、防腐性能好。
本发明所要解决的技术问题采用以下的技术方案来实现:
环氧树脂E-20 15-30,甲基三乙氧基硅烷10-15,二月桂酸二丁基锡1-3,聚酰胺固化剂1-4,硼酸3-8,钛酸丁酯3-5,纳米氧化锑锡2-7,纳米TiO2 2-4,KH-570 1-2,聚乙烯醇1-2,高岭土2-6,Sb2O3 1-2,聚磷酸铵1-4,空心玻璃微珠1-3,滑石粉1-3,MoS2粉1-3,SiC粉2-4,膨润土1-2,二甲苯、蒸馏水、HCl、无水乙醇、氨水适量。
一种含钛-硼有机硅改性环氧树脂耐磨涂料的制备方法,其特征在于,按以下步骤进行:
a. 将甲基三乙氧基硅烷、硼酸、无水乙醇混合,加入二甲苯溶解的钛酸丁酯,搅拌均匀,升温至50-70℃,加蒸馏水与HCl的混合液,调pH为3-4,保温反应1-2h,过滤,将滤液在120-140℃抽真空,得透明粘稠的液体,即为含钛-硼有机硅树脂;
b. 向环氧树脂E-20中加入二甲苯,于60-80℃水浴加热并搅拌,溶解完全后过滤,加入a中所得物料、二月桂酸二丁基锡进行混合,搅拌均匀,于130-150℃下油浴加热2-4h;
c. 室温下,向纳米氧化锑锡、纳米TiO2中加入水,磁力搅拌下加入KH-570、聚乙烯醇,用氨水调节pH至7-9,再加入MoS2粉、SiC粉,超声分散1-2h,制得浆料;
d. 将高岭土研磨水洗后于700-900℃煅烧1-2h,和Sb2O3混合,置于水中超声分散制成浆液,球磨3-5h后放入烘箱,于110-130℃干躁2-4h,得复合微粉,将其与聚磷酸铵混合均匀,待用;
e. 将b、c、d及其他剩余物料混合,研磨10-30min,加入聚酰胺固化剂,搅拌均匀,升温至95-115℃,固化1-2h,即得一种含钛-硼有机硅改性环氧树脂耐磨涂料。
本发明的反应机理如下:
(1)以甲基三乙氧基硅烷为硅源、钛酸丁酯为钛源、硼酸为硼源、HCl为催化剂,二甲苯为溶剂,二月桂酸二丁基锡为催化剂,经水解-缩合反应合成了含钛-硼有机硅树脂;硼元素的掺杂,能显著提高树脂的耐热性,有利于耐腐蚀性能的提高;所合成的掺杂钛的有机硅树脂的热稳定性最佳。
(2)纳米氧化锑锡(ATO)常用于透明隔热涂料中,具有很高的紫外红外屏蔽效果,并在可见光区具有良好的透过率,本发明通过硅烷偶联剂KH-570改性ATO粉体、纳米TiO2,再辅以分散剂聚乙烯醇分散,经过高速分散和超声波分散后,制成稳定的且分散良好的料浆,用改性环氧树脂作为成膜物,制备了透明隔热涂料。
(3)用球磨法制备了Sb2O3/高岭土复合阻燃微粉,Sb2O3属于添加型阻燃剂,以锑白粉为主,高岭土附在锑白粉表面,充分与锑白粉发生物理、化学作用;
与聚磷酸铵并用,产生协同效应,阻燃效果更佳。
(4)空心玻璃微珠内部有许多孔洞,导热系数、密度都很低,应用在涂料中能够显著的增加涂料的隔热保温效应;滑石粉表面润滑、抗粘,能提高涂层的机械力、表面硬度以及再涂覆性,主要成分为含水的硅酸镁,适用于耐高温涂料。
(5)SiC粉是耐磨涂料中常用的增强体,以SiC颗粒作为填料,有机硅改性环氧树脂为基体,制备的复合耐磨涂料能有效提高两者的界面作用。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例
一种含钛-硼有机硅改性环氧树脂耐磨涂料,由下述重量份(g)的原料制得:
环氧树脂E-20 30,甲基三乙氧基硅烷15,二月桂酸二丁基锡1,聚酰胺固化剂4,硼酸8,钛酸丁酯5,纳米氧化锑锡7,纳米TiO2 4,KH-570 2,聚乙烯醇2,高岭土6,Sb2O3 2,聚磷酸铵4,空心玻璃微珠3,滑石粉3,MoS2粉3,SiC粉4,膨润土2,二甲苯、蒸馏水、HCl、无水乙醇、氨水适量。
一种含钛-硼有机硅改性环氧树脂耐磨涂料的制备方法,其特征在于,按以下步骤进行:
a. 将甲基三乙氧基硅烷、硼酸、无水乙醇混合,加入二甲苯溶解的钛酸丁酯,搅拌均匀,升温至60-70℃,加蒸馏水与HCl的混合液,调pH为3-4,保温反应2h,过滤,将滤液在130-140℃抽真空,得透明粘稠的液体,即为含钛-硼有机硅树脂;
b. 向环氧树脂E-20中加入二甲苯,于70-80℃水浴加热并搅拌,溶解完全后过滤,加入a中所得物料、二月桂酸二丁基锡进行混合,搅拌均匀,于140-150℃下油浴加热2h;
c. 室温下,向纳米氧化锑锡、纳米TiO2中加入水,磁力搅拌下加入KH-570、聚乙烯醇,用氨水调节pH至7-8,再加入MoS2粉、SiC粉,超声分散2h,制得浆料;
d. 将高岭土研磨水洗后于800-900℃煅烧1h,和Sb2O3混合,置于水中超声分散制成浆液,球磨3h后放入烘箱,于120-130℃干躁2h,得复合微粉,将其与聚磷酸铵混合均匀,待用;
e. 将b、c、d及其他剩余物料混合,研磨30min,加入聚酰胺固化剂,搅拌均匀,升温至105-115℃,固化2h,即得一种含钛-硼有机硅改性环氧树脂耐磨涂料。
上述实施例制备的一种含钛-硼有机硅改性环氧树脂耐磨涂料的性能检测结果如下所示:
以普通碳钢为基体,用砂纸打磨,然后用无水乙醇及丙酮进行檫拭,在其表面涂覆所得涂料,放入烘箱,进行固化,涂层性能测试表明:
耐冲击性62kg.cm-1,涂层的耐沸水性5h、耐水性(25℃) 32d、耐酸性(10%HCl) 6d、耐碱性(10%NaOH) 5d、耐热性480℃、耐溶剂丙酮3d、耐盐雾31d,涂层完好,耐冷热交替性53个循环。
Claims (2)
1.一种含钛-硼有机硅改性环氧树脂耐磨涂料,其特征在于,由下述重量份的原料制得:
环氧树脂E-20 15-30,甲基三乙氧基硅烷10-15,二月桂酸二丁基锡1-3,聚酰胺固化剂1-4,硼酸3-8,钛酸丁酯3-5,纳米氧化锑锡2-7,纳米TiO2 2-4,KH-570 1-2,聚乙烯醇1-2,高岭土2-6,Sb2O3 1-2,聚磷酸铵1-4,空心玻璃微珠1-3,滑石粉1-3,MoS2粉1-3,SiC粉2-4,膨润土1-2,二甲苯、蒸馏水、HCl、无水乙醇、氨水适量。
2.根据权利要求1所述的一种含钛-硼有机硅改性环氧树脂耐磨涂料的制备方法,其特征在于,按以下步骤进行:
a. 将甲基三乙氧基硅烷、硼酸、无水乙醇混合,加入二甲苯溶解的钛酸丁酯,搅拌均匀,升温至50-70℃,加蒸馏水与HCl的混合液,调pH为3-4,保温反应1-2h,过滤,将滤液在120-140℃抽真空,得透明粘稠的液体,即为含钛-硼有机硅树脂;
b. 向环氧树脂E-20中加入二甲苯,于60-80℃水浴加热并搅拌,溶解完全后过滤,加入a中所得物料、二月桂酸二丁基锡进行混合,搅拌均匀,于130-150℃下油浴加热2-4h;
c. 室温下,向纳米氧化锑锡、纳米TiO2中加入水,磁力搅拌下加入KH-570、聚乙烯醇,用氨水调节pH至7-9,再加入MoS2粉、SiC粉,超声分散1-2h,制得浆料;
d. 将高岭土研磨水洗后于700-900℃煅烧1-2h,和Sb2O3混合,置于水中超声分散制成浆液,球磨3-5h后放入烘箱,于110-130℃干躁2-4h,得复合微粉,将其与聚磷酸铵混合均匀,待用;
e. 将b、c、d及其他剩余物料混合,研磨10-30min,加入聚酰胺固化剂,搅拌均匀,升温至95-115℃,固化1-2h,即得一种含钛-硼有机硅改性环氧树脂耐磨涂料。
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CN113488330A (zh) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | 一种功能性磁浆料的制备方法及磁性器件 |
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CN109294202A (zh) * | 2018-08-31 | 2019-02-01 | 广东国立科技股份有限公司 | 一种燃料电池专用阻燃ppo合金及其制备方法 |
CN109294202B (zh) * | 2018-08-31 | 2021-02-09 | 广东国立科技股份有限公司 | 一种燃料电池专用阻燃ppo合金及其制备方法 |
CN113488330A (zh) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | 一种功能性磁浆料的制备方法及磁性器件 |
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