CN107474910A - 一种改性蓖麻油基环保润滑脂及其制备工艺 - Google Patents

一种改性蓖麻油基环保润滑脂及其制备工艺 Download PDF

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CN107474910A
CN107474910A CN201710686049.0A CN201710686049A CN107474910A CN 107474910 A CN107474910 A CN 107474910A CN 201710686049 A CN201710686049 A CN 201710686049A CN 107474910 A CN107474910 A CN 107474910A
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castor oil
modified castor
humectation
reaction solution
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朱剑
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WUJIANG HUAWEI SPECIAL OIL Co Ltd
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Abstract

本发明公开了一种改性蓖麻油基环保润滑脂，其由以下重量份数的原料组成：改性蓖麻油100份、稠化剂12~15份、抗凝剂1~4份、耐磨合成酯5~10份、极压抗磨助剂1~4份、石墨粉3~7份、苯甲酸0.1~0.3份、烷醇酰胺0.1~0.3份、二烷基二苯胺0.1~0.3份、聚异丁烯2~4份、脂肪酸聚氧乙烯酯2~5份、羟甲基纤维素4~8份、蓖麻油烷醇酰胺硼酸酯3~6份。本发明避免了矿物基基础油的添加，最大限度的避免了润滑油脂的使用对环境造成的影响，所得润滑脂综合润滑性能良好，具有较高的经济价值和社会价值，同时适合工业化生产和使用。

Description

一种改性蓖麻油基环保润滑脂及其制备工艺
技术领域
本发明涉及润滑油脂技术领域，具体涉及一种改性蓖麻油基环保润滑脂及其制备工艺。
背景技术
随着人们的环境危机意识日益增强，人们普遍认识到现有的大量矿物基润滑油脂在生产、使用和排放过程中由于渗透、泄漏、溢出和处理不当，而造成的环境污染问题越来越严重，从社会发展的趋势来看，环保型润滑油脂将逐步取代现有的矿物基润滑油脂。
环保型润滑油脂主要以生物基润滑油脂为主，是以植物油为基础油经改性或是指在相对短的时间内可被活性微生物分解为水和二氧化碳的润滑油脂，其具有以下特点：具有良好的润滑性能，可通过节约能耗来减少环境污染；产品自身对环境无毒害、影响小；产品能被生物降解，可以分解为简单的CO2和水而被环境吸收而无危害。
环保型润滑油脂主要以植物油为主，与传统矿物润滑油相比，植物油天然的可再生和可生物降解性能可提供明显的环境和经济可持续发展的好处，而且植物油同时具有挥发性低、闪点高、粘度指数高以及润滑性优异等优势。因此，以植物油为主要来源的生物基润滑油脂就成为了环保润滑油脂的主要力量。然而，如何克服植物油氧化稳定性差、高低温性能差和抗磨损性差的问题成为了限制其作为环保润滑油脂发展的主要障碍。
发明内容
针对现有技术不足，本发明提供了一种改性蓖麻油基环保润滑脂及其制备工艺。
本发明解决上述技术问题采用的技术方案为：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂12~15份、抗凝剂1~4份、耐磨合成酯5~10份、极压抗磨助剂1~4份、石墨粉2~6份、苯甲酸0.1~0.3份、烷醇酰胺0.1~0.3份、二烷基二苯胺0.1~0.3份、聚异丁烯2~4份、脂肪酸聚氧乙烯酯2~5份、羟甲基纤维素4~8份、蓖麻油烷醇酰胺硼酸酯3~6份。
进一步地，所述改性蓖麻油制备方法，包括以下步骤：
S1: 取干燥处理后的蓖麻油置于反应容器中，加入两倍蓖麻油体积的甲苯，然后滴加1%蓖麻油体积的氢氧化钾-甲醇标准溶液，于65~70℃下保温反应30~60min，得反应液一；
S2: 将所得反应液一洗涤至中性经干燥处理后，加入三倍反应液一体积的甲苯以及732阳离子树脂和1%反应液一体积的乙酸，混匀后缓慢滴加0.5%溶液体积的H2O2，于65~70℃下反应5~7h，得反应液二；
S3: 将所得反应液二和732阳离子树脂洗涤至中性经干燥处理后，加入两倍反应液二体积的叔丁醇和3%反应液二体积的异丙醇，于65~70℃下反应5~7h，所得溶液洗涤至中性干燥后得所述改性蓖麻油。
进一步地，所述干燥处理为加入无水硫酸钠或无水氯化钙搅拌除水干燥处理。
进一步地，所述稠化剂为锂皂、钙皂或锂钙复合皂稠化剂。
进一步地，所述的抗凝剂为羟基硬脂精。
进一步地，所述的耐磨合成酯为二聚亚油酸乙二醇酯、季戊四醇四油酸酯、棕榈酸异辛酯、三羟甲基丙烷油酸酯中的一种或几种。
进一步地，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:1~3。
所述的一种改性蓖麻油基环保润滑脂的制备方法，包括以下步骤：
将稠化剂、60~80%量的改性蓖麻油加入皂化釜中混合，加热至90~120℃皂化反应1~3小时，然后加热至140~160℃后加入剩余改性蓖麻油，升温至180~200℃转移至调和釜冷却回流，冷却至90~120℃并于15~20MPa下进行均化处理，于60~90℃下加入其余原料，均化研磨、脱气处理后得到本发明的润滑脂。
蓖麻油为多种脂肪酸甘三酯的混合，其中蓖麻酸甘三酯占到约99%，其本身就有相对较好的高低温性能、抗氧化腐败性、耐水解性以及优良的电绝缘性。经改性处理的蓖麻油增加了蓖麻油的支链化，且引入了醚键，作为润滑脂的基础油粘度较低，而且绿色环保；硼酸酯类助剂的使用可以提高润滑油脂的热稳定性和阻燃性，而且具有无毒环保、可抑制可燃性气体生成和成本低的特点，在燃点高温下硼化合物分解，可在材料表面覆盖形成玻璃状焦化层，隔绝空气中氧的渗入，继而起到阻燃的作用，而且硼酸酯类添加剂具有较好的抗菌防腐性能和缓蚀性能，可大大提高润滑油脂的综合性能；聚异丁烯具有良好的粘度改性作用，且与其他组成成分协同起效，经实验测试证明具备良好的润滑效果和较强的环境适应性，非常有效的改进了生物基植物油低温流动性差的问题。
本发明避免了矿物基基础油的添加，最大限度的避免了润滑脂的使用对环境造成的影响，所得润滑脂综合润滑性能良好，具有较高的经济价值和社会价值，同时适合工业化生产和使用。
具体实施方式
下面结合具体实施例对本发明做进一步的说明，但下述的实施例并不构成对本发明权利的限制。
实施例1：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂13份、抗凝剂2份、耐磨合成酯8份、极压抗磨助剂2份、石墨粉5份、苯甲酸0.2份、烷醇酰胺0.2份、二烷基二苯胺0.2份、聚异丁烯3份、脂肪酸聚氧乙烯酯4份、羟甲基纤维素6份、蓖麻油烷醇酰胺硼酸酯5份。
进一步地，所述改性蓖麻油制备方法，包括以下步骤：
S1: 取经无水氯化钙干燥处理后的蓖麻油置于反应容器中，加入两倍蓖麻油体积的甲苯，然后滴加1%蓖麻油体积的氢氧化钾-甲醇标准溶液，于65℃下保温反应45min，得反应液一；
S2: 将所得反应液一洗涤至中性经无水硫酸钠干燥处理后，加入三倍反应液一体积的甲苯以及732阳离子树脂和1%反应液一体积的乙酸，混匀后缓慢滴加0.5%溶液体积的H2O2，于70℃下反应6h，得反应液二；
S3: 将所得反应液二和732阳离子树脂洗涤至中性经无水硫酸钠干燥处理后，加入两倍反应液二体积的叔丁醇和3%反应液二体积的异丙醇，于70℃下反应6h，所得溶液洗涤至中性经无水硫酸钠干燥后得所述改性蓖麻油。
进一步地，所述稠化剂为锂皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为二聚亚油酸乙二醇酯和三羟甲基丙烷油酸酯，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:2。
所述的一种改性蓖麻油基环保润滑脂的制备方法，包括以下步骤：
将稠化剂、70%量的改性蓖麻油加入皂化釜中混合，加热至105℃皂化反应2小时，然后加热至150℃后加入剩余改性蓖麻油，升温至190℃转移至调和釜冷却回流，冷却至105℃并于18MPa下进行均化处理，于75℃下加入其余原料，均化研磨、脱气处理后得到本发明的润滑脂。在下述的实施例中同样可以采用本实施例中所述的制备方法制备润滑脂终产品。
实施例2：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂12份、抗凝剂1份、耐磨合成酯5份、极压抗磨助剂1份、石墨粉3份、苯甲酸0.1份、烷醇酰胺0.1份、二烷基二苯胺0.1份、聚异丁烯2份、脂肪酸聚氧乙烯酯2份、羟甲基纤维素4份、蓖麻油烷醇酰胺硼酸酯3份。
进一步地，所述改性蓖麻油制备方法，包括以下步骤：
S1: 取干燥处理后的蓖麻油置于反应容器中，加入两倍蓖麻油体积的甲苯，然后滴加1%蓖麻油体积的氢氧化钾-甲醇标准溶液，于70℃下保温反应30min，得反应液一；
S2: 将所得反应液一洗涤至中性经干燥处理后，加入三倍反应液一体积的甲苯以及732阳离子树脂和1%反应液一体积的乙酸，混匀后缓慢滴加0.5%溶液体积的H2O2，于65℃下反应7h，得反应液二；
S3: 将所得反应液二和732阳离子树脂洗涤至中性经干燥处理后，加入两倍反应液二体积的叔丁醇和3%反应液二体积的异丙醇，于65℃下反应5h，所得溶液洗涤至中性干燥后得所述改性蓖麻油。
进一步地，所述干燥处理为加入无水硫酸钠或无水氯化钙搅拌除水干燥处理。
进一步地，所述稠化剂为钙皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为季戊四醇四油酸酯，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:3。
实施例3：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂15份、抗凝剂4份、耐磨合成酯10份、极压抗磨助剂4份、石墨粉7份、苯甲酸0.3份、烷醇酰胺0.3份、二烷基二苯胺0.3份、聚异丁烯4份、脂肪酸聚氧乙烯酯5份、羟甲基纤维素8份、蓖麻油烷醇酰胺硼酸酯6份。
进一步地，所述改性蓖麻油制备方法，包括以下步骤：
S1: 取干燥处理后的蓖麻油置于反应容器中，加入两倍蓖麻油体积的甲苯，然后滴加1%蓖麻油体积的氢氧化钾-甲醇标准溶液，于68℃下保温反应50min，得反应液一；
S2: 将所得反应液一洗涤至中性经干燥处理后，加入三倍反应液一体积的甲苯以及732阳离子树脂和1%反应液一体积的乙酸，混匀后缓慢滴加0.5%溶液体积的H2O2，于65℃下反应6h，得反应液二；
S3: 将所得反应液二和732阳离子树脂洗涤至中性经干燥处理后，加入两倍反应液二体积的叔丁醇和3%反应液二体积的异丙醇，于70℃下反应7h，所得溶液洗涤至中性干燥后得所述改性蓖麻油。
进一步地，所述干燥处理为加入无水硫酸钠或无水氯化钙搅拌除水干燥处理。
进一步地，所述稠化剂为锂钙复合皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为二聚亚油酸乙二醇酯、季戊四醇四油酸酯、棕榈酸异辛酯和三羟甲基丙烷油酸酯的混合，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:1。
实施例4：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂15份、抗凝剂1份、耐磨合成酯10份、极压抗磨助剂4份、石墨粉3份、苯甲酸0.3份、烷醇酰胺0.1份、二烷基二苯胺0.3份、聚异丁烯2份、脂肪酸聚氧乙烯酯5份、羟甲基纤维素4份、蓖麻油烷醇酰胺硼酸酯6份。所述的改性蓖麻油制备方法，其具体步骤同实施例1。
进一步地，所述稠化剂为锂皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为二聚亚油酸乙二醇酯和三羟甲基丙烷油酸酯，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:2。
实施例5：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：改性蓖麻油100份、稠化剂14份、抗凝剂3份、耐磨合成酯6份、极压抗磨助剂3份、石墨粉6份、苯甲酸0.1份、烷醇酰胺0.2份、二烷基二苯胺0.3份、聚异丁烯3份、脂肪酸聚氧乙烯酯3份、羟甲基纤维素5份、蓖麻油烷醇酰胺硼酸酯4份。所述的改性蓖麻油制备方法，其具体步骤同实施例1。
进一步地，所述稠化剂为锂皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为三羟甲基丙烷油酸酯，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为2:3。
对比例：一种改性蓖麻油基环保润滑脂，由以下重量份数的原料组成：精练蓖麻油100份、稠化剂13份、抗凝剂2份、耐磨合成酯8份、极压抗磨助剂2份、石墨粉5份、苯甲酸0.2份、烷醇酰胺0.2份、二烷基二苯胺0.2份、聚异丁烯3份、脂肪酸聚氧乙烯酯4份、羟甲基纤维素6份、蓖麻油烷醇酰胺硼酸酯5份。所述稠化剂为锂皂稠化剂，所述的抗凝剂为羟基硬脂精，所述的耐磨合成酯为二聚亚油酸乙二醇酯和三羟甲基丙烷油酸酯，所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:2。
取相同量的上述实施例1-5及对比例的润滑脂在相同条件下做性能测试，结果如下表所示：
性能 实施例1 实施例2 实施例3 实施例4 实施例5 对比例
滴点/℃ 254 235 267 251 262 185
氧化安定性* 0.008 0.012 0.014 0.010 0.011 0.046
生物降解性* ＞80% ＞80% ＞80% ＞80% ＞80% ＞80%
*氧化安定性（99℃，100h，0.760Mpa）压力降/Mpa。
*生物降解性：ASTMD5864。
本发明制备的一种改善低温流动性的环保润滑脂不但具有较好的润滑性、氧化稳定性和抗磨损性能，同时，本发明的润滑脂具备较好的环保性，具有较高的经济价值和社会价值。

Claims (8)

1.一种改性蓖麻油基环保润滑脂，其特征在于：由以下重量份数的原料组成：改性蓖麻油100份、稠化剂12~15份、抗凝剂1~4份、耐磨合成酯5~10份、极压抗磨助剂1~4份、石墨粉3~7份、苯甲酸0.1~0.3份、烷醇酰胺0.1~0.3份、二烷基二苯胺0.1~0.3份、聚异丁烯2~4份、脂肪酸聚氧乙烯酯2~5份、羟甲基纤维素4~8份、蓖麻油烷醇酰胺硼酸酯3~6份。
2.根据权利要求1所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述改性蓖麻油制备方法，包括以下步骤：
S1: 取干燥处理后的蓖麻油置于反应容器中，加入两倍蓖麻油体积的甲苯，然后滴加1%蓖麻油体积的氢氧化钾-甲醇标准溶液，于65~70℃下保温反应30~60min，得反应液一；
S2: 将所得反应液一洗涤至中性经干燥处理后，加入三倍反应液一体积的甲苯以及732阳离子树脂和1%反应液一体积的乙酸，混匀后缓慢滴加0.5%溶液体积的H2O2，于65~70℃下反应5~7h，得反应液二；
S3: 将所得反应液二和732阳离子树脂洗涤至中性经干燥处理后，加入两倍反应液二体积的叔丁醇和3%反应液二体积的异丙醇，于65~70℃下反应5~7h，所得溶液洗涤至中性干燥后得所述改性蓖麻油。
3.根据权利要求2所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述干燥处理为加入无水硫酸钠或无水氯化钙搅拌除水干燥处理。
4.根据权利要求1所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述稠化剂为锂皂、钙皂或锂钙复合皂稠化剂。
5.根据权利要求1所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述的抗凝剂为羟基硬脂精。
6.根据权利要求1所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述的耐磨合成酯为二聚亚油酸乙二醇酯、季戊四醇四油酸酯、棕榈酸异辛酯、三羟甲基丙烷油酸酯中的一种或几种。
7.根据权利要求1所述的一种改性蓖麻油基环保润滑脂，其特征在于：所述极压抗磨助剂为蓖麻油烷醇酰胺硼酸酯和二烷基二硫代氨基甲酸钼的复合物，其质量份比为1:1~3。
8.权利要求1-7任一项所述的一种改性蓖麻油基环保润滑脂的制备工艺，其特征在于，包括以下步骤：将稠化剂、60~80%量的改性蓖麻油加入皂化釜中混合，加热至90~120℃皂化反应1~3小时，然后加热至140~160℃后加入剩余改性蓖麻油，升温至180~200℃转移至调和釜冷却回流，冷却至90~120℃并于15~20MPa下进行均化处理，于60~90℃下加入其余原料，均化研磨、脱气处理后得到本发明的润滑脂。
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Application publication date: 20171215