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CN108559612B - 一种皂基润滑剂的制备方法 - Google Patents

一种皂基润滑剂的制备方法 Download PDF

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CN108559612B
CN108559612B CN201810352251.4A CN201810352251A CN108559612B CN 108559612 B CN108559612 B CN 108559612B CN 201810352251 A CN201810352251 A CN 201810352251A CN 108559612 B CN108559612 B CN 108559612B
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陈文�
卢志敏
刘保
蔡熙扬
沈平
何辉
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Guangzhou Langqi Daily Necessities Co ltd
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Abstract

本发明的目的在于提供一种皂基润滑剂的制备方法，所述的制备方法条件温和，反应时间短，能有效提高反应的效率，降低能耗。本发明将油脂乳化成水包油包水的乳液，达到微乳化效果，乳液的粒径为50～100nm，使油脂在进行皂化反应之前已得到充分的分散，在皂化反应中增加油脂与碱液接触的表面积，利于反应的进行。在皂化过程中，不会发生破乳，只是中间层物质发生改变，反应结束后，油脂层变为脂肪酸皂层，反应前被油脂层包裹的水层被脂肪酸皂包裹，均匀分布在脂肪酸皂内层，成为润滑剂的胶溶剂。

Description

一种皂基润滑剂的制备方法
技术领域
本发明属于润滑剂领域，尤其涉及一种皂基润滑剂的制备方法。
背景技术
皂基润滑剂为脂肪酸皂作稠化剂的润滑脂。常见的有钙基、无水钙基、复合钙基、复合磺酸钙基、钠基胺钠基、铝基、复合铝基、锂基、复合锂基等润滑脂。钙钠基、钡基和铅基润滑脂已被淘汰。由于各种脂肪酸的特性不同，所制得润滑脂的使用性能也各异。
润滑脂有90％是以脂肪酸皂作稠化剂，即以脂肪或脂肪酸与碱发生皂化反应制成。常用的脂肪和脂肪酸有牛油、猪油、棉子油、硬脂酸,12-羧基硬脂酸等，也有采用氧化石蜡制成的合成脂肪酸，但效果不及天然脂肪酸。所用的碱类则多为碱金属和碱土金属的氢氧化物，如氢氧化钠、氢氧化钙、氢氧化锂等。
皂基润滑剂因对机械部件具有良好的润滑及防护作用，而被广泛应用。但在现有技术中，常规的油脂皂化工艺需要高温长时间的反应，一般皂化温度需要大于100℃，皂化时间至少3～4小时，反应效率低，能耗高，无法适应当前日益增长的润滑剂需求。因此，有必要研发一种皂化条件温和、皂化时间短的皂基润滑剂。
发明内容
本发明的目的是提供一种皂基润滑剂的制备方法，所述的制备方法条件温和，反应时间短，能有效提高反应的效率，降低能耗。
本发明通过以下技术方案实现：
一种皂基润滑剂的制备方法，包含以下步骤：
1)将油脂、HLB值＜6的乳化剂混合均匀，得到油相，将水、多元醇混合均匀，得到水相A，在充分搅拌后，将水相A缓慢加入油相中继续搅拌进行乳化，得到乳液a，乳液a为油包水结构的乳液；
2)将多元醇、HLB值＞15的乳化剂、水混合均匀，得到水相B，将步骤1)所得的乳液a在搅拌下加入到水相B中继续搅拌进行乳化，得到乳液b，乳液b为水包油包水结构的乳液；
3)将氢氧化钾、水混合得到氢氧化钾溶液，然后将步骤2)得到的乳液b在搅拌下加入到氢氧化钾溶液中进行皂化反应，得到皂基润滑剂。
优选地，所述步骤1)将40～48％油脂、3～5％HLB值＜6的乳化剂混合均匀，得到油相，将3～5％水、4～6％多元醇混合均匀，得到水相A；更优选地，所述步骤1)将42～46％油脂、3.5～4％HLB值＜6的乳化剂混合均匀，得到油相，将3.5～4％水、5～5.5％多元醇混合均匀，得到水相A。
优选地，步骤1)所述水相A在1000～1200rpm的搅拌速度下充分搅拌后，将水相A缓慢加入油相中继续搅拌进行乳化，乳化温度为40～50℃，乳化时间为25～35min，得到乳液a，乳液a为油包水结构的乳液。
优选地，所述步骤2)将4～6％多元醇、2～3％HLB值＞15的乳化剂、7～12％水混合均匀，得到水相B；更优选地，所述步骤2)将4.5～5％多元醇、2～3％HLB值＞15的乳化剂、8～10％水混合均匀，得到水相B。
优选地，步骤2)所述乳液a在600～800rpm的搅拌速度下加入到水相B中继续搅拌进行乳化，乳化温度为30～40℃，乳化时间为20～30min，得到乳液b，乳液b为水包油包水结构的乳液。
优选地，所述步骤3)将10～15％氢氧化钾、10～15％水混合得到氢氧化钾溶液；更优选地，所述步骤3)将11～13％氢氧化钾、13～15％水混合得到氢氧化钾溶液。
优选地，步骤3)所述乳液b在600～800rpm的搅拌速度下加入到氢氧化钾溶液中进行皂化反应，保持反应温度为40～50℃，反应50～80min。
以上所述的百分比均是组分质量占制备所述皂基润滑剂所需原料总质量的百分比。
优选地，所述多元醇为丙二醇、甘油、山梨醇中的一种或两种以上的复配。
本发明的原理是：通过先将步骤1)所述水相A缓慢加入油相中进行搅拌乳化，形成油包水结构的乳液a；然后在步骤2)中将乳液a缓慢加入水相B中进行搅拌乳化，进一步形成水包油包水结构的乳液，达到微乳化效果，乳液的粒径为50～100nm，使油脂在进行皂化反应之前已得到充分的分散，在皂化反应中增加油脂与碱液接触的表面积，利于反应的进行。在皂化过程中，不会发生破乳，只是中间层物质发生改变，反应结束后，油脂层变为脂肪酸皂层，反应前被油脂层包裹的水层被脂肪酸皂包裹，水均匀分布在脂肪酸皂内层，成为润滑剂的胶溶剂。本发明由于制备工艺与现有技术不同，使得润滑剂的微观结构与常规皂基润滑剂不同，性能也获得了大幅度的提升。
本发明与现有技术相比具有以下有益效果：
1.油脂在皂化反应前微乳化形成水包油包水结构的乳液，得到充分的分散，在皂化反应中增加油脂与碱液接触的表面积，提高反应速率，从现有技术的3～4小时缩短至95～145分钟，且使得皂化反应在温和的反应条件下更容易进行，从现有技术大于100℃的反应温度下降至30～50℃；
2.本发明在皂化过程中不会出现破乳而破坏水包油包水的乳液结构，在反应过程中仅中间层物质发生改变，反应结束后，油脂层变为脂肪酸皂层，反应前被油脂层包裹的水层被脂肪酸皂包裹，均匀分布在脂肪酸皂内层，成为润滑剂的胶溶剂，被包裹的水分难以蒸发，降低润滑剂的蒸发度，使润滑剂更为稳定，提高高温条件下的使用性能；
3.乳液状态使润滑剂具有更好的粘附性，可以更好地粘附在机器设备上，同时具有更好的流动性，减少机器运转时的阻力，减少功率的损耗。
具体实施方式
以下通过具体的实施例对本发明作进一步的阐述。
本发明所述的实施例中，使用的油脂为椰子油、蓖麻油、棉籽油、棕榈油、棕榈仁油、菜油、牛羊油中的一种或多种的混合物；HLB值＜6的乳化剂选自月桂醇聚氧乙烯醚-2、月桂醇聚氧乙烯醚-3、月桂醇聚氧乙烯醚-7、月桂醇聚氧乙烯醚-9、斯盘-80、斯盘-60中的一种或两种以上的复配，HLB值＞15的乳化剂选自聚醚L35、月桂醇硫酸钠、油酸钠、吐温-20中的一种或两种以上的复配，使用的多元醇选自丙二醇、甘油、山梨醇中的一种或两种以上的复配。
本发明各实施例中的所述的皂基润滑剂通过以下方法制备：
1)将油脂、HLB值＜6的乳化剂混合均匀，得到油相，将水、多元醇混合均匀，得到水相A，在充分搅拌后，将水相A缓慢加入油相中继续搅拌进行乳化，得到乳液a，乳液a为油包水结构的乳液；
2)将多元醇、HLB值＞15的乳化剂、水混合均匀，得到水相B，将步骤1)所得的乳液a在搅拌下加入到水相B中继续搅拌进行乳化，得到乳液b，乳液b为水包油包水结构的乳液；
3)将氢氧化钾、水混合得到氢氧化钾溶液，然后将步骤2)得到的乳液b在搅拌下加入到氢氧化钾溶液中进行皂化反应，得到皂基润滑剂。
各实施例的具体的组分及制备的反应条件如下表-1所示：
表-1
Figure BDA0001633681640000041
Figure BDA0001633681640000051
将实施例2所制得的皂基润滑剂与常规皂化法合成的润滑剂进行对比测试，测试结果如下表-2所示。
表-2
Figure BDA0001633681640000052
Figure BDA0001633681640000061
从表-2的对比测试结果可见，相比于常规皂化法合成的润滑剂，实施例2合成的皂基润滑剂具有更高的滴点，耐温性能更好；分油率低，高温条件下的胶体安定性好，在机器运作过程中不容易出现分油现象；蒸发量低，氧化安定性好，水淋流失量低，更加稳定；相似粘度低，在机器运行过程中摩擦损失小，润滑性能更好。
实施例1、实施例3～6所制得的皂基润滑剂经检测后得到与实施例2相近的结果。本发明所述的油脂可以在椰子油、蓖麻油、棉籽油、棕榈油、棕榈仁油、菜油、牛羊油等各种动植物油中的一种或多种的混合物之间自由替换；所述HLB＜6的乳化剂可以在月桂醇聚氧乙烯醚-2、月桂醇聚氧乙烯醚-3、月桂醇聚氧乙烯醚-7、月桂醇聚氧乙烯醚-9、斯盘-80、斯盘-60等各种乳化剂中的一种或两种以上的复配之间自由替换；HLB＞15的乳化剂可以在聚醚L35、月桂醇硫酸钠、油酸钠、吐温-20等各种乳化剂中的一种或两种以上的复配之间自由替换；所述的多元醇可以丙二醇、甘油、山梨醇等多元醇中的一种或两种以上的复配之间自由替换。上述的自由替换均能使制得的皂基润滑剂达到相近的效果。
应当指出的是，上述的具体实施例仅是对本发明的进一步说明而不是限制，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种皂基润滑剂的制备方法，其特征在于，包含以下步骤：
1)将油脂、HLB值＜6的乳化剂混合均匀，得到油相；将水、多元醇混合均匀，得到水相A，在充分搅拌后，将水相A缓慢加入油相中继续搅拌进行乳化，得到乳液a，乳液a为油包水结构的乳液；
2)将多元醇、HLB值＞15的乳化剂、水混合均匀，得到水相B；将步骤1)所得的乳液a在搅拌下加入到水相B中继续搅拌进行乳化，得到乳液b，乳液b为水包油包水结构的乳液；
3)将氢氧化钾、水混合得到氢氧化钾溶液；然后将步骤2)得到的乳液b在搅拌下加入到氢氧化钾溶液中进行皂化反应，得到皂基润滑剂。
2.根据权利要求1所述的皂基润滑剂的制备方法，其特征在于，所述步骤1)将40～48％油脂、3～5％HLB值＜6的乳化剂混合均匀，得到油相；将3～5％水、4～6％多元醇混合均匀，得到水相A；以上所述的百分比均是组分质量占制备所述皂基润滑剂所需原料总质量的百分比。
3.根据权利要求2所述的皂基润滑剂的制备方法，其特征在于，所述步骤1)将42～46％油脂、3.5～4％HLB值＜6的乳化剂混合均匀，得到油相；将3.5～4％水、5～5.5％多元醇混合均匀，得到水相A。
4.根据权利要求1～3任一项所述的皂基润滑剂的制备方法，其特征在于，步骤1)所述水相A在1000～1200rpm的搅拌速度下充分搅拌后，将水相A缓慢加入油相中继续搅拌进行乳化，乳化温度为40～50℃，乳化时间为25～35min，得到乳液a，乳液a为油包水结构的乳液。
5.根据权利要求1所述的皂基润滑剂的制备方法，其特征在于，所述步骤2)将4～6％多元醇、2～3％HLB值＞15的乳化剂、7～12％水混合均匀，得到水相B；以上所述的百分比均是组分质量占制备所述皂基润滑剂所需原料总质量的百分比。
6.根据权利要求5所述的皂基润滑剂的制备方法，其特征在于，所述步骤2)将4.5～5％多元醇、2～3％HLB值＞15的乳化剂、8～10％水混合均匀，得到水相B。
7.根据权利要求1、5、6任一项所述的皂基润滑剂的制备方法，其特征在于，步骤2)所述乳液a在600～800rpm的搅拌速度下加入到水相B中继续搅拌进行乳化，乳化温度为30～40℃，乳化时间为20～30min，得到乳液b，乳液b为水包油包水结构的乳液。
8.根据权利要求1所述的皂基润滑剂的制备方法，其特征在于，所述步骤3)将10～15％氢氧化钾、10～15％水混合得到氢氧化钾溶液；以上所述的百分比均是组分质量占制备所述皂基润滑剂所需原料总质量的百分比。
9.根据权利要求8所述的皂基润滑剂的制备方法，其特征在于，所述步骤3)将11～13％氢氧化钾、13～15％水混合得到氢氧化钾溶液。
10.根据权利要求1、8、9任一项所述的皂基润滑剂的制备方法，其特征在于，步骤3)所述乳液b在600～800rpm的搅拌速度下加入到氢氧化钾溶液中进行皂化反应，保持反应温度为40～50℃，反应50～80min。
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