CN106635337A - 一种柔韧环保型α‑D‑呋喃葡萄糖改性硅酸锂水基防锈液及其制备方法 - Google Patents

一种柔韧环保型α‑D‑呋喃葡萄糖改性硅酸锂水基防锈液及其制备方法 Download PDF

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CN106635337A
CN106635337A CN201611157529.XA CN201611157529A CN106635337A CN 106635337 A CN106635337 A CN 106635337A CN 201611157529 A CN201611157529 A CN 201611157529A CN 106635337 A CN106635337 A CN 106635337A
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江海涛
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Tianchang Runda Metal Antirust Auxiliary Co Ltd
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Abstract

本发明公开了一种柔韧环保型α‑D‑呋喃葡萄糖改性硅酸锂水基防锈液，由下列重量份的原料制成：埃洛石纳米管2.3‑2.5、甲基丙烯酸甲酯0.7‑0.9、过硫酸钠0.05‑0.07、硅酸锂1.2‑1.5、十二烯基丁二酸50‑55、三乙醇胺20‑22、OP‑10 30‑33、磷酸锌15‑16、纳米结晶纤维素1.2‑1.6、硅烷偶联剂kh‑550 0.4‑0.6、羟丙基瓜尔胶0.8‑1.2、乙醇5‑5.5。本发明通过使用纳米结晶纤维素、硅烷偶联剂kh‑550、羟丙基瓜尔胶、乙醇形成均一稳定分散液，能够在金属表面形成致密、柔韧、光亮的薄膜，提高防锈性能，瓜尔胶对水分子的捕获能力,防锈膜的热稳定性有所改善。

Description

一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液及其 制备方法
技术领域
本发明涉及防锈液技术领域，尤其涉及一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液及其制备方法。
背景技术
为了满足金属切削液的防锈添加剂应用中清洁环保的要求,以获得无硫磷并具有优良减摩抗磨作用的高性能防锈剂为目的,本论文采用羟基保护与脱保护的制备工艺,根据防锈剂作用原理,分别设计、制备了四种α-D-呋喃葡萄糖的3-位取代衍生物水基防锈剂:3-苯甲酰基-α-D-呋喃葡萄糖、3-苄基-α-D-呋喃葡萄糖、3-乙酰基-α-D-呋喃葡萄糖和3-十二酰基-α-D-呋喃葡萄糖。以3-苯甲酰基-α-D-呋喃葡萄糖、3-苄基-α-D-呋喃葡萄糖、3-乙酰基-α-D-呋喃葡萄糖、3-十二酰基-α-D-呋喃葡萄糖、壳牌复合防锈剂和油酸的5%水溶液为研究试样。使用四球摩擦磨损试验机对6个试样进行摩擦磨损性能的测试,结果表明这四种多羟基葡萄糖衍生物水基防锈剂具有较好的减摩抗磨性能,减摩抗磨效果明显优于油酸,略低于壳牌复合防锈剂。使用球棒抗疲劳试验机对6个试样进行抗疲劳磨损试验,结果表明这四种多羟基葡萄糖衍生物水基防锈剂的抗疲劳特征寿命是油酸的2～4倍,最大特征寿命的可以达到192.2min,低于壳牌复合防锈剂的256.4min。采用行业标准SH0365-92对6个试样与水进行单片防锈试验,结果表明这四种多羟基葡萄糖衍生物水基防锈剂的防锈时间比油酸提高5～8倍,其中3-苯甲酰基-α-D-呋喃葡萄糖、3-苄基-α-D-呋喃葡萄糖和3-十二酰基-α-D-呋喃葡萄糖的防锈时间高于壳牌复合防锈剂。采用CS350电化学工作站对6个试样进行电化学性能试验,测试样品自腐蚀电位和腐蚀电流密度,结果表明这四种多羟基葡萄糖衍生物水基防锈剂没有引起阳极和阴极Tafel常数明显变化;与空白样对比,自腐蚀电位均向阳极方向移动;四种多羟基葡萄糖衍生物缓的蚀效率均＞80%,其中3-苄基-α-D-呋喃葡萄糖和3-十二酰基-α-D-呋喃葡萄糖的缓蚀效率可以达到93%以上,高于壳牌复合防锈剂的87.9%。
金属件通常防锈的手段为镀镍、镀铬等,但由于成本等因素,电镀企业一般会尽量减少镀层厚度,造成镀件防锈性能降低,需借助涂覆防锈剂补充防锈。研究了以低浓度硅酸锂溶液为主,与多种不同的助剂复配,配制低浓度环保型水基防锈液。并采用正交实验确定了防锈液的最佳配比为:硅酸锂浓度为0.012mol/L,有机酸添加量为0.5mL/L,有机胺添加量为0.2g/L,磷酸盐添加量为0.15g/L,OP-10添加量为0.3mL/L。在最佳配比条件下,防锈液防锈性能良好,无毒环保,性能稳定,60d后仍有理想的防锈效果。
《低浓度环保型硅酸锂水基防锈液的研究》一文得到的防锈液不能形成致密的膜，防锈时间较短，需要改进，利用α-D-呋喃葡萄糖成膜性好，易降解，与硅酸锂溶液结合，改善防锈液的防锈性能还未见报道，还需要提高防锈液的柔韧性，防开裂脱落。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液及其制备方法。
本发明是通过以下技术方案实现的：
一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液，由下列重量份的原料制成：埃洛石纳米管2.3-2.5、甲基丙烯酸甲酯0.7-0.9、过硫酸钠0.05-0.07、硅酸锂1.2-1.5、十二烯基丁二酸50-55、三乙醇胺20-22、OP-10 30-33、磷酸锌15-16、水适量、二氯甲烷适量、无水硫酸钠36-39、α-D-呋喃葡萄糖5-6、浓硫酸5.3-6.5、丙酮45-50、氢氧化钠6.5-7、纳米结晶纤维素1.2-1.6、硅烷偶联剂kh-550 0.4-0.6、羟丙基瓜尔胶0.8-1.2、乙醇5-5.5。
所述柔韧保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液的制备方法，包括以下步骤：
（1）将α-D-呋喃葡萄糖加入容器再放入冰浴中，滴加浓硫酸，保持温度在5℃以下搅拌2-2.5h，加入丙酮，在20-22℃下搅拌5-6h，用氢氧化钠中和，过滤，用二氯甲烷洗涤滤饼3次，加入无水硫酸钠干燥，过滤，将滤液旋蒸，得到中间体；
（2）将埃洛石纳米管分散在8-10重量份水中，加入1/3的甲基丙烯酸甲酯、过硫酸钠，搅拌均匀，加热至80-83℃，再加入中间体，搅拌反应20-25分钟，再加入剩余的甲基丙烯酸甲酯、过硫酸钠，继续反应40-50分钟，得到改性α-D-呋喃葡萄糖；
（3）将硅烷偶联剂kh-550分散在乙醇中，再加入羟丙基瓜尔胶，超声分散4-5分钟，再加入纳米结晶纤维素，加热至60-65℃，超声分散4-5分钟，得到悬浮液；
（4）按硅酸锂0.012-0.014mol/L、十二烯基丁二酸0.5-0.6mL/L、三乙醇胺0.2-0.3g/L、OP-10 0.3-0.4mL/L、磷酸锌0.15g/L的浓度配制水溶液，再加入改性α-D-呋喃葡萄糖、悬浮液，混合均匀，即得。
本发明的优点是：本发明使用埃洛石纳米管与α-D-呋喃葡萄糖进行接枝改性，提高了α-D-呋喃葡萄糖的分散性，在金属表面形成致密的防锈薄膜，还能够吸附防锈成分起到缓蚀作用，提高了防锈效果，α-D-呋喃葡萄糖的降解性好，减少了环境污染；通过使用纳米结晶纤维素、硅烷偶联剂kh-550、羟丙基瓜尔胶、乙醇形成均一稳定分散液，能够在金属表面形成致密、柔韧、光亮的薄膜，提高防锈性能，瓜尔胶对水分子的捕获能力,复合膜的水蒸气阻隔性能提高了,防锈膜的热稳定性也有所改善。
具体实施方式
一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液，由下列重量份（公斤）的原料制成：埃洛石纳米管2.3、甲基丙烯酸甲酯0.7、过硫酸钠0.05、硅酸锂1.2、十二烯基丁二酸50、三乙醇胺20、OP-10 30、磷酸锌15、水适量、二氯甲烷适量、无水硫酸钠36、α-D-呋喃葡萄糖5、浓硫酸5.3、丙酮45、氢氧化钠6.5、纳米结晶纤维素1.2、硅烷偶联剂kh-550 0.4、羟丙基瓜尔胶0.8、乙醇5。
所述柔韧保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液的制备方法，包括以下步骤：
（1）将α-D-呋喃葡萄糖加入容器再放入冰浴中，滴加浓硫酸，保持温度在5℃以下搅拌2h，加入丙酮，在20℃下搅拌5h，用氢氧化钠中和，过滤，用二氯甲烷洗涤滤饼3次，加入无水硫酸钠干燥，过滤，将滤液旋蒸，得到中间体；
（2）将埃洛石纳米管分散在8重量份水中，加入1/3的甲基丙烯酸甲酯、过硫酸钠，搅拌均匀，加热至80℃，再加入中间体，搅拌反应20分钟，再加入剩余的甲基丙烯酸甲酯、过硫酸钠，继续反应40分钟，得到改性α-D-呋喃葡萄糖；
（3）将硅烷偶联剂kh-550分散在乙醇中，再加入羟丙基瓜尔胶，超声分散4分钟，再加入纳米结晶纤维素，加热至60℃，超声分散4分钟，得到悬浮液；
（4）按硅酸锂0.012mol/L、十二烯基丁二酸0.5mL/L、三乙醇胺0.2g/L、OP-10 0.3mL/L、磷酸锌0.15g/L的浓度配制水溶液，再加入改性α-D-呋喃葡萄糖、悬浮液，混合均匀，即得。
实验数据：
将在75g蒸馏水中加入5g亚铁氰化钾和20gNaCl，搅拌溶解，用检测液浸湿滤纸，将滤纸包贴在烘干后的镀件上，1min后，滤纸上没有蓝点，防锈性能合格。滤纸包覆2min后观察腐蚀面积为0.19mm2,70天后防锈油仍然清澈不浑浊，具有理想的防锈效果。

Claims (2)

1.一种柔韧环保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液，其特征在于：由下列重量份的原料制成：埃洛石纳米管2.3-2.5、甲基丙烯酸甲酯0.7-0.9、过硫酸钠0.05-0.07、硅酸锂1.2-1.5、十二烯基丁二酸50-55、三乙醇胺20-22、OP-10 30-33、磷酸锌15-16、水适量、二氯甲烷适量、无水硫酸钠36-39、α-D-呋喃葡萄糖5-6、浓硫酸5.3-6.5、丙酮45-50、氢氧化钠6.5-7、纳米结晶纤维素1.2-1.6、硅烷偶联剂kh-550 0.4-0.6、羟丙基瓜尔胶0.8-1.2、乙醇5-5.5。
2.根据权利要求1所述柔韧保型α-D-呋喃葡萄糖改性硅酸锂水基防锈液的制备方法，其特征在于包括以下步骤：
（1）将α-D-呋喃葡萄糖加入容器再放入冰浴中，滴加浓硫酸，保持温度在5℃以下搅拌2-2.5h，加入丙酮，在20-22℃下搅拌5-6h，用氢氧化钠中和，过滤，用二氯甲烷洗涤滤饼3次，加入无水硫酸钠干燥，过滤，将滤液旋蒸，得到中间体；
（2）将埃洛石纳米管分散在8-10重量份水中，加入1/3的甲基丙烯酸甲酯、过硫酸钠，搅拌均匀，加热至80-83℃，再加入中间体，搅拌反应20-25分钟，再加入剩余的甲基丙烯酸甲酯、过硫酸钠，继续反应40-50分钟，得到改性α-D-呋喃葡萄糖；
（3）将硅烷偶联剂kh-550分散在乙醇中，再加入羟丙基瓜尔胶，超声分散4-5分钟，再加入纳米结晶纤维素，加热至60-65℃，超声分散4-5分钟，得到悬浮液；
（4）按硅酸锂0.012-0.014mol/L、十二烯基丁二酸0.5-0.6mL/L、三乙醇胺0.2-0.3g/L、OP-10 0.3-0.4mL/L、磷酸锌0.15g/L的浓度配制水溶液，再加入改性α-D-呋喃葡萄糖、悬浮液，混合均匀，即得。
CN201611157529.XA 2016-12-15 2016-12-15 一种柔韧环保型α‑D‑呋喃葡萄糖改性硅酸锂水基防锈液及其制备方法 Pending CN106635337A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108728836A (zh) * 2018-06-05 2018-11-02 陈太师 一种高效防锈剂
IT201700122757A1 (it) * 2017-10-27 2019-04-27 Univ Degli Studi Di Palermo A composition comprising a cellulose nanofiber and halloysite nanotube, a film, and a composite comprising the same
CN111575096A (zh) * 2020-06-15 2020-08-25 许卫明 防锈变速箱机油及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201700122757A1 (it) * 2017-10-27 2019-04-27 Univ Degli Studi Di Palermo A composition comprising a cellulose nanofiber and halloysite nanotube, a film, and a composite comprising the same
CN108728836A (zh) * 2018-06-05 2018-11-02 陈太师 一种高效防锈剂
CN111575096A (zh) * 2020-06-15 2020-08-25 许卫明 防锈变速箱机油及其制备方法

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