CN110484327A - 一种防硬化的钙基滚动轴承润滑脂的制备 - Google Patents

一种防硬化的钙基滚动轴承润滑脂的制备 Download PDF

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CN110484327A
CN110484327A CN201810478731.5A CN201810478731A CN110484327A CN 110484327 A CN110484327 A CN 110484327A CN 201810478731 A CN201810478731 A CN 201810478731A CN 110484327 A CN110484327 A CN 110484327A
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acid
base oil
temperature
preparation
calcium
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万同
江华欣
刘书文
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Tianjin University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
    • C10M123/02—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a non-macromolecular compound
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or salts
    • C10M2201/0856—Phosphorus oxides, acids or salts used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087—Boron oxides, acids or salts
    • C10M2201/0876—Boron oxides, acids or salts used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
    • C10M2207/1225—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic used as thickening agent
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

本发明设计了一种防硬化钙基滚动类轴承润滑脂的制备方法及所制得的产品。该制备过程是：以基础油、硬脂酸、氢氧化钙、冰乙酸、磷酸和硼酸为主要原料，在润滑油相中反应制得产品。按顺序包括以下步骤：(1)将硬脂酸与基础油混合并加热，当温度升至80～90℃时加入氢氧化钙进行皂化反应，皂化温度维持在100～105℃；(2)升温使温度维持在110～140℃，加入冰乙酸、磷酸和硼酸进行复合1小时；(3)升温至180℃，进行高温炼制；(4)加入剩余基础油，升温至220℃并保温一段时间后冷却降温，研磨，得到最终产品。本发明方法所得产品具有较高的滴点且放置一个月无明显硬化现象。

Description

一种防硬化的钙基滚动轴承润滑脂的制备
技术领域
本发明涉及化学合成和润滑脂制备技术领域，具体涉及一种防硬化钙基滚动轴承润滑脂合成制备方法及所制得的产品。
背景技术
润滑脂是一种稠厚的油脂状半固体，用于机械的摩擦部分，起润滑和密封作用。也用于金属表面，起填充空隙和防锈作用。随着现代工业的飞速发展，对润滑材料的要求日益苛刻，高负荷、高速、低噪音下机械设备需要连续运转，润滑脂的应用温度需达到200℃以上高温，要求润滑脂具有较高的滴点、良好的抗水性、对金属表面有较好的粘附性；同时不随存放时间而出现硬化和不易析油。目前使用的复合钙基润滑脂制备工艺会出现自身的严重硬化问题，同时滴点不高，难以满足实际的使用要求。
本发明要解决的问题
传统的钙基润滑脂生产方法是将硬脂酸和石灰乳分别加入到基础油中进行反应并加入乙酸复合为乙酸钙，控制稠化炼制温度制得钙基润滑脂。但乙酸钙容易分解为醋酸而挥发形成碳酸钙使润滑脂在储存过程中和高温使用条件下产生表面硬化现象，并影响润滑脂的使用性能。与传统的钙基润滑脂制备方法不同的是本发明利用两种无机酸配比替代部分的乙酸反应得到润滑脂来改善其硬化现象。
发明内容
本发明提供了一种防硬化的钙基的润滑脂的制备方法。
由于醋酸钙不稳定容易造成润滑脂的硬化。本发明利用磷酸和硼酸配比替代部分乙酸有效解决其硬化问题。
制备方法如下步骤：
1)在反应釜中将硬脂酸以一定的摩尔比例范围投料，并加入基础油搅拌加热到80～90℃，确保硬脂酸完全溶解于基础油溶解完成后保温10～20min；
2)在反应釜中将氢氧化钙以一定的摩尔比例范围分批加入至基础油中并加入适量的水混合搅拌加热到100～105℃，皂化完成后保温20～30min，确保皂化过程中没有溢釜；
3)升温至反应釜中温度为110～140℃，在反应釜中缓慢加入一定比例范围的冰乙酸、磷酸和硼酸进行复合。
4)加完酸后保温20～30min再升温到180℃并保温20～30min，完成后再加入一定量的基础油并升温到210～220℃进行高温炼制，完成后保温一段时间，后经过滤器过滤移入中间釜进行冷却。冷却到130℃以下，将润滑脂用三辊分散机研磨，得到产品。
本发明的有益效果是：
采用本发明制备的过程，采用磷酸和硼酸配比替代部分冰乙酸有效解决其硬化问题。所制得的润滑脂满足较高的滴点要求。
具体实施方式
下面结合具体的实施例对本发明进行进一步的说明。
实施例1：
将100g基础油和18g硬脂酸加入到反应釜中，搅拌加热到80℃；再将9.75g氢氧化钙和适量的水加入反应釜中进行皂化，搅拌加热到100℃，皂化保温20min，在110～140℃将3g冰乙酸、3g磷酸和1.03g硼酸缓慢滴加到反应釜中进行复合，反应0.5小时；完成后快速升温至160～180℃，加入25g基础油，升温至220℃并保温20min，降温至130℃以下。再将润滑脂用三辊分散机进行研磨，得到产品。
性能测试结果：滴点300℃，放置一个月无明显硬化。
实施例2：
将100g基础油和18g硬脂酸加入到反应釜中，搅拌加热到80℃；再将9.75g氢氧化钙和适量的水加入反应釜中进行皂化，搅拌加热到100℃，皂化保温20min，在100～140℃将4.6g才乙酸和4.4g硼酸和0.6g磷酸缓慢滴加到反应釜中进行复合，反应0.5小时；完成后快速升温至160～180℃，加入25g基础油，升温至220℃并保温20min，降温至130℃以下。再将润滑脂用三辊分散机进行研磨，得到产品。
性能测试结果：滴点320℃，放置一个月无明显硬化。

Claims (2)

1.一种防硬化的钙基滚动类轴承润滑脂的制备方法。其合成制备反应的特征在于：将硬脂酸和氢氧化钙以一定的摩尔比例范围完全溶解于基础油加入反应釜进行皂化反应。皂化反应加入冰乙酸、磷酸和硼酸进行复合，控制反应温度和时间，最后加入剩余基础油再升温到220℃后进行冷却降温。
2.根据权利要求1所述的制备方法中氢氧化钙与硬脂酸的摩尔比百分数分别为0.55～2之间。冰乙酸与无机酸(磷酸和硼酸)进行复合质量比例范围为1∶1～3之间。磷酸和硼酸质量比例范围为1∶0.3～3之间。
CN201810478731.5A 2018-05-15 2018-05-15 一种防硬化的钙基滚动轴承润滑脂的制备 Pending CN110484327A (zh)

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