CN106928836B - 一种铝合金用硼酸化水性聚氨酯钝化液的制备方法 - Google Patents

一种铝合金用硼酸化水性聚氨酯钝化液的制备方法 Download PDF

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CN106928836B
CN106928836B CN201710184540.3A CN201710184540A CN106928836B CN 106928836 B CN106928836 B CN 106928836B CN 201710184540 A CN201710184540 A CN 201710184540A CN 106928836 B CN106928836 B CN 106928836B
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张龙
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Abstract

本发明公开了一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,本发明的硼酸化水性聚氨酯钝化液可以在铝合金基材表面形成均匀稳定的润滑膜,加入的硅溶胶还可以增强涂膜与基材的附着力,提高表面强度,可以对铝合金起到长久的保护,本发明采用聚氨酯为主要成膜物质,其形成的涂膜粘接牢固、柔韧性及弹性好、可以更有效地阻止腐蚀介质对铝层侵蚀,提高铝板的耐蚀性,具有长期优异的防锈、防刮擦性能,且本发明为无铬钝化液,使用安全,环保性好。

Description

一种铝合金用硼酸化水性聚氨酯钝化液的制备方法
技术领域
本发明属于材料领域,具体涉及一种铝合金用硼酸化水性聚氨酯钝化液的制备方法。
背景技术
传统的表面钝化工艺以铬酸盐为主,由于六价铬有致癌性,正逐渐被禁用。目前的无铬钝化技术主要包括硅酸盐、钼酸盐等无机钝化,植酸、单宁酸等有机钝化。然而,单纯的无机膜或有机膜的耐蚀性能仍无法取代铬酸盐。而有机/无机复合钝化液具有协同作用可提高钝化膜的耐蚀性,如将水性环氧树脂、镍盐、双氧水及有机酸等配制成复合钝化液,所得钝化膜的耐蚀性较好,但由于其固化剂为反应型,复合后钝化液的存储、施工都很麻烦;水溶性丙烯酸树脂中加入少量钼酸盐和磷酸盐得到复合钝化液,所得钝化膜可推迟镀锌层出现白锈的时间,但附着力和韧性差,且有裂纹,常用的聚丙烯酸酯膜抗粘连性差,容易出现热黏冷脆的现象,因此为了不断提高铝合金的钝化效果,需要研究一种新的环保性好、附着力高、成膜性好、防腐蚀性好的高品质钝化液。
发明内容
本发明的目的在于针对现有技术的缺陷和不足,提供一种环保性好、附着力高、成膜性好、防腐蚀性好的铝合金用硼酸化水性聚氨酯钝化液的制备方法。
为实现上述目的,本发明采用以下技术方案:
一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,其特征在于,包括以下步骤:
(1)取石油磺酸钡,加入到其重量30-40倍的无水乙醇中,搅拌均匀;
(2)取正硅酸乙酯,加入到其重量60-100倍的去离子水中,搅拌均匀,滴加浓度为10-15%的氨水,调节pH为11-12,搅拌1-2小时,加入上述石油磺酸钡的乙醇溶液,升高温度为70-76℃,保温搅拌50-60分钟,得硅溶胶;
(3)取2,2-二溴-3-氰基丙酰胺,加入到其重量20-30倍的去离子水中,搅拌均匀,与上述硅溶胶混合,超声3-5分钟,得酰胺溶胶分散液;
(4)取硼酸、2,2-二甲基丙醇混合,送入到反应釜中,通入氮气,在80-110℃下保温反应100-120分钟,加入二月桂酸二丁基锡,继续升高温度为150-160℃,保温反应6-8小时,出料冷却,真空40-50℃下干燥1-2小时,得硼酸化聚酯多元醇;
(5)取聚丙二醇ppg1000,在110-120℃下真空脱水2-3小时,降低温度至55-60℃,与上述硼酸化聚酯多元醇混合,搅拌均匀,加入异佛尔酮二异氰酸酯,在55-60℃下保温搅拌20-30分钟,送入到反应釜中,通入氮气,加入辛酸亚锡,升高温度为80-85℃,保温反应5-6小时,加入1,4丁二醇,搅拌至常温,冷却出料,得硼酸化溶胶聚氨酯预聚体;
(6)取羧甲基纤维素钠、硅酸钠混合,加入到上述酰胺溶胶分散液中,升高温度为60-70℃,加入上述硼酸化溶胶聚氨酯预聚体,1800-2000转/分搅拌20-30分钟,加入二甲基硅油,搅拌至常温,得所述铝合金用硼酸化水性聚氨酯钝化液。
所述的石油磺酸钡、正硅酸乙酯、2,2-二溴-3-氰基丙酰胺、硼酸、2,2-二甲基丙醇、二月桂酸二丁基锡、聚丙二醇ppg1000、异佛尔酮二异氰酸酯、辛酸亚锡、1,4丁二醇、羧甲基纤维素钠、硅酸钠、二甲基硅油的重量比为3-4:15-20:1-2:10-14:15-20:0.4-0.6:80-90:100-110:2-3:4-5:1-2:10-12:1-3。
本发明钝化液在使用时还可以加入适量的水调稀,将铝合金基材脱脂除油,反复水洗,在本发明的钝化液中浸泡处理,时间为3-20分钟,出料后将铝合金基材进行烘干,烘干温度为60-70℃,干燥时间为20-40分钟,即可。
本发明的优点:
本发明首先采用防腐蚀剂石油磺酸钡分散到乙醇中,之后将得到的醇分散液参与到以正硅酸乙酯为前驱体的水解反应中,得到具有抗锈性的硅溶胶,然后再通过酰胺分散,与无机防锈剂硅酸钠混合,进一步提高溶胶分散液的抗锈性能,然后采用硼酸为酸性单体,二月桂酸二丁基锡为催化剂,得到硼酸化聚酯多元醇,然后与聚丙二醇ppg1000单体混合,参与到聚氨酯的反应中,在反应结束时,引入1.4丁二醇作为扩链剂,得到可以在水中有效分散的聚合物,最后将该聚合物分散到具有抗锈功能的溶胶分散液中,得到最终产物,本发明的硼酸化水性聚氨酯钝化液可以在铝合金基材表面形成均匀稳定的润滑膜,加入的硅溶胶还可以增强涂膜与基材的附着力,提高表面强度,可以对铝合金起到长久的保护,本发明采用聚氨酯为主要成膜物质,其形成的涂膜粘接牢固、柔韧性及弹性好、可以更有效地阻止腐蚀介质对铝层侵蚀,提高铝板的耐蚀性,具有长期优异的防锈、防刮擦性能,且本发明为无铬钝化液,使用安全,环保性好。
具体实施方式
实施例1
一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,包括以下步骤:
(1)取石油磺酸钡,加入到其重量40倍的无水乙醇中,搅拌均匀;
(2)取正硅酸乙酯,加入到其重量100倍的去离子水中,搅拌均匀,滴加浓度为15%的氨水,调节pH为12,搅拌1-2小时,加入上述石油磺酸钡的乙醇溶液,升高温度为70-76℃,保温搅拌60分钟,得硅溶胶;
(3)取2,2-二溴-3-氰基丙酰胺,加入到其重量30倍的去离子水中,搅拌均匀,与上述硅溶胶混合,超声5分钟,得酰胺溶胶分散液;
(4)取硼酸、2,2-二甲基丙醇混合,送入到反应釜中,通入氮气,在110℃下保温反应120分钟,加入二月桂酸二丁基锡,继续升高温度为160℃,保温反应8小时,出料冷却,真空50℃下干燥2小时,得硼酸化聚酯多元醇;
(5)取聚丙二醇ppg1000,在120℃下真空脱水3小时,降低温度至55-60℃,与上述硼酸化聚酯多元醇混合,搅拌均匀,加入异佛尔酮二异氰酸酯,在60℃下保温搅拌30分钟,送入到反应釜中,通入氮气,加入辛酸亚锡,升高温度为85℃,保温反应6小时,加入1,4丁二醇,搅拌至常温,冷却出料,得硼酸化溶胶聚氨酯预聚体;
(6)取羧甲基纤维素钠、硅酸钠混合,加入到上述酰胺溶胶分散液中,升高温度为70℃,加入上述硼酸化溶胶聚氨酯预聚体,2000转/分搅拌30分钟,加入二甲基硅油,搅拌至常温,得所述铝合金用硼酸化水性聚氨酯钝化液。
所述的石油磺酸钡、正硅酸乙酯、2,2-二溴-3-氰基丙酰胺、硼酸、2,2-二甲基丙醇、二月桂酸二丁基锡、聚丙二醇ppg1000、异佛尔酮二异氰酸酯、辛酸亚锡、1,4丁二醇、羧甲基纤维素钠、硅酸钠、二甲基硅油的重量比为4:20:1:14:20:0.6:90:110:3:5:2:12:3。
性能测试:
取铝合金试片,脱脂除油,反复水洗,在本发明的钝化液中浸泡处理,时间为10分钟,出料后将铝合金试片进行烘干,烘干温度为60℃,干燥时间为17分钟,对其进行中性盐雾试验24小时,腐蚀面积为1.1%。
实施例2
一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,包括以下步骤:
(1)取石油磺酸钡,加入到其重量30倍的无水乙醇中,搅拌均匀;
(2)取正硅酸乙酯,加入到其重量60倍的去离子水中,搅拌均匀,滴加浓度为10%的氨水,调节pH为11,搅拌1小时,加入上述石油磺酸钡的乙醇溶液,升高温度为70℃,保温搅拌50分钟,得硅溶胶;
(3)取2,2-二溴-3-氰基丙酰胺,加入到其重量20-30倍的去离子水中,搅拌均匀,与上述硅溶胶混合,超声3分钟,得酰胺溶胶分散液;
(4)取硼酸、2,2-二甲基丙醇混合,送入到反应釜中,通入氮气,在80℃下保温反应100分钟,加入二月桂酸二丁基锡,继续升高温度为150℃,保温反应6小时,出料冷却,真空40℃下干燥1小时,得硼酸化聚酯多元醇;
(5)取聚丙二醇ppg1000,在110℃下真空脱水2小时,降低温度至55-60℃,与上述硼酸化聚酯多元醇混合,搅拌均匀,加入异佛尔酮二异氰酸酯,在55℃下保温搅拌20分钟,送入到反应釜中,通入氮气,加入辛酸亚锡,升高温度为80℃,保温反应5小时,加入1,4丁二醇,搅拌至常温,冷却出料,得硼酸化溶胶聚氨酯预聚体;
(6)取羧甲基纤维素钠、硅酸钠混合,加入到上述酰胺溶胶分散液中,升高温度为60℃,加入上述硼酸化溶胶聚氨酯预聚体,1800转/分搅拌20分钟,加入二甲基硅油,搅拌至常温,得所述铝合金用硼酸化水性聚氨酯钝化液。
所述的石油磺酸钡、正硅酸乙酯、2,2-二溴-3-氰基丙酰胺、硼酸、2,2-二甲基丙醇、二月桂酸二丁基锡、聚丙二醇ppg1000、异佛尔酮二异氰酸酯、辛酸亚锡、1,4丁二醇、羧甲基纤维素钠、硅酸钠、二甲基硅油的重量比为3:15:1:10:15:0.4:80:100:2:4-1:10:1。
性能测试:
取铝合金试片,脱脂除油,反复水洗,在本发明的钝化液中浸泡处理,时间为10分钟,出料后将铝合金试片进行烘干,烘干温度为60℃,干燥时间为17分钟,对其进行中性盐雾试验24小时,腐蚀面积为0.8%;
可以看出,本发明的钝化液具有很好的耐腐蚀性能。

Claims (2)

1.一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,其特征在于,包括以下步骤:
(1)取石油磺酸钡,加入到其重量30-40倍的无水乙醇中,搅拌均匀;
(2)取正硅酸乙酯,加入到其重量60-100倍的去离子水中,搅拌均匀,滴加浓度为10-15%的氨水,调节pH为11-12,搅拌1-2小时,加入上述石油磺酸钡的乙醇溶液,升高温度为70-76℃,保温搅拌50-60分钟,得硅溶胶;
(3)取2,2-二溴-3-氰基丙酰胺,加入到其重量20-30倍的去离子水中,搅拌均匀,与上述硅溶胶混合,超声3-5分钟,得酰胺溶胶分散液;
(4)取硼酸、2,2-二甲基丙醇混合,送入到反应釜中,通入氮气,在80-110℃下保温反应100-120分钟,加入二月桂酸二丁基锡,继续升高温度为150-160℃,保温反应6-8小时,出料冷却,真空40-50℃下干燥1-2小时,得硼酸化聚酯多元醇;
(5)取聚丙二醇ppg1000,在110-120℃下真空脱水2-3小时,降低温度至55-60℃,与上述硼酸化聚酯多元醇混合,搅拌均匀,加入异佛尔酮二异氰酸酯,在55-60℃下保温搅拌20-30分钟,送入到反应釜中,通入氮气,加入辛酸亚锡,升高温度为80-85℃,保温反应5-6小时,加入1,4-丁二醇,搅拌至常温,冷却出料,得硼酸化溶胶聚氨酯预聚体;
(6)取羧甲基纤维素钠、硅酸钠混合,加入到上述酰胺溶胶分散液中,升高温度为60-70℃,加入上述硼酸化溶胶聚氨酯预聚体,1800-2000转/分搅拌20-30分钟,加入二甲基硅油,搅拌至常温,得所述铝合金用硼酸化水性聚氨酯钝化液。
2.根据权利要求1所述的一种铝合金用硼酸化水性聚氨酯钝化液的制备方法,其特征在于,所述的石油磺酸钡、正硅酸乙酯、2,2-二溴-3-氰基丙酰胺、硼酸、2,2-二甲基丙醇、二月桂酸二丁基锡、聚丙二醇ppg1000、异佛尔酮二异氰酸酯、辛酸亚锡、1,4-丁二醇、羧甲基纤维素钠、硅酸钠、二甲基硅油的重量比为3-4:15-20:1-2:10-14:15-20:0.4-0.6:80-90:100-110:2-3:4-5:1-2:10-12:1-3。
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