CN107974162B - 一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法 - Google Patents
一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法 Download PDFInfo
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Abstract
本发明公开了一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，将滑石粉、磷酸锌、三聚磷酸铝混合，加分散剂、钛酸酯偶联剂和去离子水，分散研磨得颜料浆液；将纳米二氧化硅烘干后与聚乙二醇、甲苯混合，加热回流反应得聚乙二醇接枝改性纳米粒子；向云母氧化铁中加甲苯，搅拌、超声得A组分；将甲苯二异氰酸酯、二丁基二月桂酸锡、甲苯混匀，滴加到A组分中搅拌反应，再升温反应得甲苯二异氰酸酯改性云母氧化铁填料；向苯酚中加甲醛水溶液、蒸馏水、草酸，将混合物回流搅拌，再加草酸搅拌回流，加蒸馏水静置分层，将上层液体加热减压蒸馏，加混合溶剂，得到酚醛清漆树脂，加固化剂及前面所得物料，搅匀得所述酚醛树脂漆。
Description
技术领域
本发明涉及涂料领域，具体涉及一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法。
背景技术
涂层防护法是防止金属腐蚀最有效、应用最广泛的方法，而环氧树脂是目前应用最广泛的防腐涂料，但由于环氧涂料自身性脆、易老化等缺点，环氧树脂类涂料是重要的有机涂料之一，但其韧性及耐高温性能不佳，通常需要对其改性。云母氧化铁是防锈颜料的主要品种之一，呈薄片状结晶，耐热性高。以云母氧化铁制成的涂料具有良好的形成膜、优良的附着力和连接特性、抗大气污染和紫外光无辐射、极佳的耐久性及容易涂装成厚膜等特点。三聚磷酸铝作为一种新型无毒防 锈颜料，除了具有耐水性好、抗蚀性强的特点之外，还能增强阻燃、减震、抗压、耐磨等性能，所以广泛应用于不同树脂制成金属板材防护用防腐蚀涂料，是目前最具应用前景的防锈颜料。
发明内容
本发明主要解决的技术问题是提供一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，依照该方法制备的涂料具有良好耐磨防腐性能和防锈性能。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，按以下步骤进行：
（1）颜填料的表面改性处理：
将12-18重量份滑石粉、8-13重量份磷酸锌、8-13重量份三聚磷酸铝混合，加入2-6重量份分散剂、0.5-1重量份钛酸酯偶联剂和去离子水，用分散磨砂机研磨1-2h，制得颜料浆液；
（2）接枝聚乙二醇法改性纳米二氧化硅：
将4-6重量份纳米二氧化硅在115-120℃真空烘箱中烘2-3h，然后与14-16重量份聚乙二醇、85-90重量份甲苯混合，超声振荡30-35min，磁力搅拌下加热至108-112℃回流反应2-3h，离心、用乙醇洗涤3-5次，在120-125℃真空烘箱中烘1-2h，得到聚乙二醇接枝改性纳米粒子；
（3）云母氧化铁的改性：
向4-6重量份云母氧化铁中加入80-90重量份甲苯，搅拌30-35min后超声处理20-25min，得A组分；在氮气保护下，将2-4重量份甲苯二异氰酸酯、0.05-0.1重量份二丁基二月桂酸锡、40-45重量份甲苯混匀，然后滴加到A组分中，高速搅拌反应1-2h后，升温至88-92℃继续反应5-6h，过滤、甲苯洗涤3-5次，得到甲苯二异氰酸酯改性的云母氧化铁填料；
（4）酚醛树脂涂料的制备：
向60-70重量份苯酚中加入40-50重量份甲醛水溶液、6-7重量份去离子水、0.4-0.6重量份草酸，将混合物在78-82℃下回流搅拌30-35min，再加入0.4-0.6重量份草酸，继续搅拌回流1-2h，然后加入190-210重量份去离子水，静置分层，将上层液体加热至115-125℃减压蒸馏，加入混合溶剂，得到含量为48-52%的酚醛清漆树脂，加入5-7重量份固化剂六次甲基四胺及(1)、(2)、(3)中所得物料，搅拌混合均匀，得到所述酚醛树脂漆。
其中，步骤（1）中分散剂为SP-762，钛酸酯偶联剂为TC-311，研磨速度为3000-3500rpm，颜填料的体积浓度为20-25%。步骤（2）中聚乙二醇分子量为1000。步骤（3）中滴加速度为10-15滴/min。步骤（4）中甲醛水溶液的浓度为35-40%，混合溶剂为乙醇:丁醇以体积比3:1混合。
本发明的反应机理及有益效果如下：
以滑石粉、磷酸锌、三聚磷酸铝为防锈颜填料，用分散剂、钛酸酯偶联剂对其表面进行改性处理，可改善防锈颜料的表面状况及其在涂料体系中的分散效果，防锈颜料在涂料中分散更均匀，偶联剂起到连接高分子树脂与无机颗粒的“桥梁”的作用，长效防锈效果好；用聚乙二醇为改性剂与纳米二氧化硅粒子表面羟基进行醇酯化反应，接枝改性后纳米粒子在溶剂中分散性好，添加到涂料中可改善涂层的附着力，接枝聚乙二醇法改性纳米二氧化硅复合涂料的耐磨性能佳，也可改善涂层的耐水性能；以云母氧化铁为防锈颜料，用甲苯二异氰酸酯对其进行改性，改善其在涂层中的分散性，且平行于金属表面的片层增多，可降低涂层的吸水率；将所制得的颜料浆液、聚乙二醇接枝改性纳米粒子、甲苯二异氰酸酯改性的云母氧化铁填料添加到酚醛涂料中，可得到一种防锈防水耐磨型涂料。
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
一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，按以下步骤进行：
（1）颜填料的表面改性处理：
将12kg滑石粉、8kg磷酸锌、8kg三聚磷酸铝混合，加入2kg分散剂、0.5kg钛酸酯偶联剂和去离子水，用分散磨砂机研磨1h，制得颜料浆液；
（2）接枝聚乙二醇法改性纳米二氧化硅：
将4kg纳米二氧化硅在115-120℃真空烘箱中烘2h，然后与14kg聚乙二醇、85-90kg甲苯混合，超声振荡35min，磁力搅拌下加热至108-112℃回流反应3h，离心、用乙醇洗涤3次，在120-125℃真空烘箱中烘2h，得到聚乙二醇接枝改性纳米粒子；
（3）云母氧化铁的改性：
向4kg云母氧化铁中加入80kg甲苯，搅拌35min后超声处理25min，得A组分；在氮气保护下，将2kg甲苯二异氰酸酯、0.05kg二丁基二月桂酸锡、40kg甲苯混匀，然后滴加到A组分中，高速搅拌反应1h后，升温至88-92℃继续反应5h，过滤、甲苯洗涤3次，得到甲苯二异氰酸酯改性的云母氧化铁填料；
（4）酚醛树脂涂料的制备：
向60kg苯酚中加入40kg甲醛水溶液、6kg去离子水、0.4kg草酸，将混合物在78-82℃下回流搅拌35min，再加入0.4kg草酸，继续搅拌回流1h，然后加入190kg去离子水，静置分层，将上层液体加热至115-125℃减压蒸馏，加入混合溶剂，得到含量为48-52%的酚醛清漆树脂，加入5kg固化剂六次甲基四胺及(1)、(2)、(3)中所得物料，搅拌混合均匀，得到所述酚醛树脂漆。
其中，步骤（1）中分散剂为SP-762，钛酸酯偶联剂为TC-311，研磨速度为3500rpm，颜填料的体积浓度为20%。步骤（2）中聚乙二醇分子量为1000。步骤（3）中滴加速度为15滴/min。步骤（4）中甲醛水溶液的浓度为35%，混合溶剂为乙醇:丁醇以体积比3:1混合。
Claims (5)
1.一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，按以步骤进行：
（1）颜填料的表面改性处理：
将12-18重量份滑石粉、8-13重量份磷酸锌、8-13重量份三聚磷酸铝混合，加入2-6重量份分散剂、0.5-1重量份钛酸酯偶联剂和去离子水，用分散磨砂机研磨1-2h，制得颜料浆液；
（2）接枝聚乙二醇法改性纳米二氧化硅：
将4-6重量份纳米二氧化硅在115-120℃真空烘箱中烘2-3h，然后与14-16重量份聚乙二醇、85-90重量份甲苯混合，超声振荡30-35min，磁力搅拌下加热至108-112℃回流反应2-3h，离心、用乙醇洗涤3-5次，在120-125℃真空烘箱中烘1-2h，得到聚乙二醇接枝改性纳米粒子；
（3）云母氧化铁的改性：
向4-6重量份云母氧化铁中加入80-90重量份甲苯，搅拌30-35min后超声处理20-25min，得A组分；在氮气保护下，将2-4重量份甲苯二异氰酸酯、0.05-0.1重量份二丁基二月桂酸锡、40-45重量份甲苯混匀，然后滴加到A组分中，高速搅拌反应1-2h后，升温至88-92℃继续反应5-6h，过滤、甲苯洗涤3-5次，得到甲苯二异氰酸酯改性的云母氧化铁填料；
（4）酚醛树脂涂料的制备：
向60-70重量份苯酚中加入40-50重量份甲醛水溶液、6-7重量份去离子水、0.4-0.6重量份草酸，将混合物在78-82℃下回流搅拌30-35min，再加入0.4-0.6重量份草酸，继续搅拌回流1-2h，然后加入190-210重量份去离子水，静置分层，将上层液体加热至115-125℃减压蒸馏，加入混合溶剂，得到含量为48-52%的酚醛清漆树脂，加入5-7重量份固化剂六次甲基四胺及(1)、(2)、(3)中所得物料，搅拌混合均匀，得到所述酚醛树脂漆。
2. 根据权利要求1所述的一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，步骤（1）中分散剂为SP-762，钛酸酯偶联剂为TC-311，研磨速度为3000-3500rpm，颜填料的体积浓度为20-25%。
3.根据权利要求1所述的一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，步骤（2）中聚乙二醇分子量为1000。
4.根据权利要求1所述的一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，步骤（3）中滴加速度为10-15滴/min。
5. 根据权利要求1所述的一种云母氧化铁改性的防锈防水耐磨型酚醛树脂漆的制备方法，其特征在于，步骤（4）中甲醛水溶液的浓度为35-40%，混合溶剂为乙醇:丁醇以体积比3: 1混合。
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