CN109504503A - 一种链条润滑脂及其制备方法 - Google Patents
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Abstract
本发明提供了一种链条润滑脂,其特征在于,按重量份称取以下成分:改性蚕蛹油基础油55‑70份,矿物基础油15‑30份,脂肪酸锂皂20‑40份,硫化异丁烯1‑3份,磷酸三甲酚酯1‑3份,纳米石墨4‑6份,抗氧化剂T204为1‑4份;其中改性蚕蛹油基础油通过精制,预酯化,乙酯化和环氧化得到。本发明通过以蚕蛹为原料,通过提取静置蚕蛹油,在通过乙酯化,环氧化,开环反应制备得到环境友好型润滑脂基础油,并与适量的矿物油相混合,经性能测试,表现出润滑性能稳定,使用周期较长,耐磨性和高温稳定性好。
Description
技术领域
本发明涉及润滑油领域,具体涉及一种链条润滑脂及其制备方法。
背景技术
链条在工业方面有长期和广泛的应用,常用的有传动链条、传送链条、举升链条和控制链条等。链条的磨损主要发生在销轴与套筒之间,磨损使得间隙变大、链条变长直到链条不能准确的与链轮啮合,或者不能维持正确的定距与定时。有时辊子与套筒之间的磨损或链板与导板之间的磨损也会导致链条故障。
工业传动链条的润滑以链条油为主,少数使用润滑脂,链条油由基础油与添加剂组成。脂油;是酸与醇类反应的产物,用作润滑剂的主要有双脂和多元醇脂。脂油的优点是温度范围宽、抗氧化性好、矿物油兼容性好。缺点是成本较高、水解稳定性差。
随着现代生产的迅速发展,经济迅速膨胀,严峻的能源问题也随之而来。根据研究,按照目前的能源使用效率,地球上总石油储量仅可维持使用四十多年,天然气的储量仅够使用五十年左右。目前在西方许多发达国家能源问题已经成为制约经济发展的一个重要原因,解决能源危机问题最直接、最有效的的方法是使用可再生能源来代替目前的石油产品;另一方面,随着全球对大气环境及水土污染的高度重视,人们也逐渐开始在大气污染控制方面投入越来越多的人力、物力及财力,以解决环境污染给人类带来的一系列威胁。对于润滑油而言,传统的矿物油基润滑油由于生物降解性差,已不能满足人类保护环境的需要。综上所述,研究与开发代用润滑剂势在必行,也是很有发展前景的领域。
发明内容
要解决的技术问题:本发明的目的是提供一种链条用润滑脂,成本低,选用工业蚕蛹油与矿物油混合制备得到,润滑作用好,承载能力强和耐高温性能佳。
技术方案:一种链条润滑脂,按重量份称取以下成分:改性蚕蛹油基础油55-70份,矿物基础油15-30份,脂肪酸锂皂20-40份,硫化异丁烯1-3份,磷酸三甲酚酯1-3份,纳米石墨4-6份,抗氧化剂T204为1-4份;其中改性蚕蛹油基础油通过精制,预酯化,乙酯化和环氧化得到。
进一步的,所述改性蚕蛹油基础油的制备方法包括以下步骤:
S1. 干燥后的蚕蛹用粉碎机粉碎,过40目筛,超临界CO2萃取:压力20-30 MPa、温度40-50℃、时间 1-2.5 h,获得蚕蛹毛油,然后通过脱胶和脱酸制备得到精制蚕蛹油;
S2. 将蚕蛹油预热至65-75℃,然后加入浓硫酸和无水乙醇,在机械搅拌下加热回流1-2h ,将产物,洗涤,减压旋蒸,去水,得到预酯化的蚕蛹油;
S3. 将步骤S2制备的蚕蛹油预热至65-75℃,然后加入氢氧化钾和乙醇,加热回流反应1-2h,静置分层,提纯得到乙酯化的蚕蛹油;
S4. 在步骤S3制备的乙酯化的蚕蛹油中加入甲酸和对甲苯磺酸,升温至50-60℃后,滴加双氧水,一边滴加双氧水,边升温至100℃,即停止反应,静置分层,分离提纯上层油相,得到环氧化蚕蛹油。
进一步的,所述步骤S1中脱胶的方法为:将蚕蛹毛油水浴加热到70℃,缓慢加入占油质量1%的磷酸,反应充分后,离心分别获得上层脱胶油。
进一步的,所述步骤S1中脱酸的方法为:向脱胶蛹油中加入3 moL/L的NaOH溶液,缓慢滴加并均匀搅拌加热到70 ℃保温30 min,冷却至室温,分离,提纯油相,得到精制蛹油。
上述的一种链条润滑脂的制备方法,将改性蚕蛹油基础油和矿物基础油混合均与后,加入脂肪酸锂皂在110-140℃进行炼制1-3h,再150-160℃下脱水1h,降温至80℃,加入剩余的成分,继续搅拌20-40min,研磨脱泡得到链条润滑脂。
进一步的,所述矿物基础油为500SN矿物油。
有益效果:本发明通过以蚕蛹为原料,通过提取静置蚕蛹油,在通过乙酯化,环氧化,开环反应制备得到环境友好型润滑脂基础油,并与适量的矿物油相混合,经性能测试,表现出润滑性能稳定,使用周期较长,耐磨性和高温稳定性好。
具体实施方式
实施例1
改性蚕蛹油基础油的制备方法包括以下步骤:
S1. 干燥后的蚕蛹用粉碎机粉碎,过40目筛,超临界CO2萃取:压力20 MPa、温度40℃、时间 1h,获得蚕蛹毛油,然后通过脱胶和脱酸制备得到精制蚕蛹油;
S2. 将蚕蛹油预热至65℃,然后加入浓硫酸和无水乙醇,在机械搅拌下加热回流1h ,将产物,洗涤,减压旋蒸,去水,得到预酯化的蚕蛹油,其中蚕蛹油:浓硫酸:无水乙醇的质量比10:0.5:1;
S3. 将步骤S2制备的蚕蛹油预热至65℃,然后加入氢氧化钾和乙醇,加热回流反应2h,静置分层,提纯得到乙酯化的蚕蛹油,其中蚕蛹油:氢氧化钾:乙醇的质量比为10:1.5:1;
S4. 在步骤S3制备的乙酯化的蚕蛹油中加入甲酸和对甲苯磺酸,升温至50℃后,滴加双氧水,一边滴加双氧水,边升温至100℃,即停止反应,静置分层,分离提纯上层油相,得到环氧化蚕蛹油,其中蚕蛹油:甲酸:双氧水的质量比为20:4:50。
实施例2
改性蚕蛹油基础油的制备方法包括以下步骤:
S1. 干燥后的蚕蛹用粉碎机粉碎,过40目筛,超临界CO2萃取:压力30 MPa、温度50℃、时间 2.5 h,获得蚕蛹毛油,然后通过脱胶和脱酸制备得到精制蚕蛹油;
S2. 将蚕蛹油预热至75℃,然后加入浓硫酸和无水乙醇,在机械搅拌下加热回流2h ,将产物,洗涤,减压旋蒸,去水,得到预酯化的蚕蛹油,其中蚕蛹油:浓硫酸:无水乙醇的质量比10:1:1;
S3. 将步骤S2制备的蚕蛹油预热至75℃,然后加入氢氧化钾和乙醇,加热回流反应1h,静置分层,提纯得到乙酯化的蚕蛹油,其中蚕蛹油:氢氧化钾:乙醇的质量比为10:0.5:1;
S4. 在步骤S3制备的乙酯化的蚕蛹油中加入甲酸和对甲苯磺酸,升温至60℃后,滴加双氧水,一边滴加双氧水,边升温至100℃,即停止反应,静置分层,分离提纯上层油相,得到环氧化蚕蛹油,其中蚕蛹油:甲酸:双氧水的质量比为25:3:50。
实施例3
改性蚕蛹油基础油的制备方法包括以下步骤:
S1. 干燥后的蚕蛹用粉碎机粉碎,过40目筛,超临界CO2萃取:压力25 MPa、温度45℃、时间 1.5 h,获得蚕蛹毛油,然后通过脱胶和脱酸制备得到精制蚕蛹油;
S2. 将蚕蛹油预热至70℃,然后加入浓硫酸和无水乙醇,在机械搅拌下加热回流1.5h,将产物,洗涤,减压旋蒸,去水,得到预酯化的蚕蛹油,其中蚕蛹油:浓硫酸:无水乙醇的质量比10:0.8:1;
S3. 将步骤S2制备的蚕蛹油预热至70℃,然后加入氢氧化钾和乙醇,加热回流反应2h,静置分层,提纯得到乙酯化的蚕蛹油,其中蚕蛹油:氢氧化钾:乙醇的质量比为10:1:1;
S4. 在步骤S3制备的乙酯化的蚕蛹油中加入甲酸和对甲苯磺酸,升温至55℃后,滴加双氧水,一边滴加双氧水,边升温至100℃,即停止反应,静置分层,分离提纯上层油相,得到环氧化蚕蛹油,其中蚕蛹油:甲酸:双氧水的质量比为22:4:50。
实施例1-3中蚕蛹毛油的脱胶和脱酸的制备方法为:
脱胶:将蚕蛹毛油水浴加热到70℃,缓慢加入占油质量1%的磷酸,反应充分后,离心分别获得上层脱胶油;
脱酸:向脱胶蛹油中加入3 moL/L的NaOH溶液,缓慢滴加并均匀搅拌加热到70 ℃保温30 min,冷却至室温,分离,提纯油相,得到精制蛹油。
实施例4
一种链条润滑脂,按重量份称取以下成分:实施例1制得的改性蚕蛹油基础油55份,500SN矿物基础油30份,脂肪酸锂皂20份,硫化异丁烯3份,磷酸三甲酚酯1份,纳米石墨4份,抗氧化剂T204为4份;
一种链条润滑脂的制备方法,将改性蚕蛹油基础油和矿物基础油混合均与后,加入脂肪酸锂皂在140℃进行炼制1h,再150℃下脱水1h,降温至80℃,加入剩余的成分,继续搅拌20min,研磨脱泡得到链条润滑脂。
实施例5
一种链条润滑脂,按重量份称取以下成分:实施例2制得的改性蚕蛹油基础油70份,500SN矿物基础油15份,脂肪酸锂皂40份,硫化异丁烯1份,磷酸三甲酚酯3份,纳米石墨6份,抗氧化剂T204为1份;
一种链条润滑脂的制备方法,将改性蚕蛹油基础油和矿物基础油混合均与后,加入脂肪酸锂皂在110℃进行炼制3h,再160℃下脱水1h,降温至80℃,加入剩余的成分,继续搅拌40min,研磨脱泡得到链条润滑脂。
实施例6
一种链条润滑脂,按重量份称取以下成分:实施例3制得的改性蚕蛹油基础油65份,500SN矿物基础油20份,脂肪酸锂皂30份,硫化异丁烯2份,磷酸三甲酚酯2份,纳米石墨5份,抗氧化剂T204为3份;
一种链条润滑脂的制备方法,将改性蚕蛹油基础油和矿物基础油混合均与后,加入脂肪酸锂皂在130℃进行炼制2h,再160℃下脱水1h,降温至80℃,加入剩余的成分,继续搅拌30min,研磨脱泡得到链条润滑脂。
对比例为将实施例6中的改性蚕蛹油基础油等量替换为500SN矿物基础油,其余步骤均相同。
下表为本发明制备的润滑脂的实施例和对比例的性能比较。
性能指标 | 测试标准 | 实施例4 | 实施例5 | 实施例6 | 对比例 |
滴点(℃) | GB/T 3498 | 296 | 288 | 292 | 256 |
润滑寿命(h) | 在150℃下,1000r/min,204轴承 | 808 | 800 | 810 | 602 |
锥入度(200℃,24h),0.1mm | GB/T 269 | 303 | 312 | 310 | 254 |
极压性能(最大无卡咬负荷PB值)N | GB/T 12583 | 802 | 789 | 805 | 671 |
极压性能(烧结负荷PD值)N | GB/T 12583 | 3256 | 3129 | 3211 | 2535 |
四球墨痕实验(392N,1200r/min,75,1h)磨痕直径mm | 0.25 | 0.28 | 0.24 | 0.22 | 0.46 |
Claims (6)
1.一种链条润滑脂,其特征在于,按重量份称取以下成分:改性蚕蛹油基础油55-70份,矿物基础油15-30份,脂肪酸锂皂20-40份,硫化异丁烯1-3份,磷酸三甲酚酯1-3份,纳米石墨4-6份,抗氧化剂T204为1-4份;其中改性蚕蛹油基础油通过精制,预酯化,乙酯化和环氧化得到。
2.根据权利要求1所述的一种链条润滑脂,其特征在于,所述改性蚕蛹油基础油的制备方法包括以下步骤:
S1. 干燥后的蚕蛹用粉碎机粉碎,过40目筛,超临界CO2萃取:压力20-30 MPa、温度40-50℃、时间 1-2.5 h,获得蚕蛹毛油,然后通过脱胶和脱酸制备得到精制蚕蛹油;
S2. 将蚕蛹油预热至65-75℃,然后加入浓硫酸和无水乙醇,在机械搅拌下加热回流1-2h ,将产物,洗涤,减压 旋蒸,去水,得到预酯化的蚕蛹油;
S3. 将步骤S2制备的蚕蛹油预热至65-75℃,然后加入氢氧化钾和乙醇,加热回流反应1-2h,静置分层,提纯得到乙酯化的蚕蛹油;
S4. 在步骤S3制备的乙酯化的蚕蛹油中加入甲酸和对甲苯磺酸,升温至50-60℃后,滴加双氧水,一边滴加双氧水,边升温至100℃,即停止反应,静置分层,分离提纯上层油相,得到环氧化蚕蛹油。
3.根据权利要求2所述的一种链条润滑脂,其特征在于,所述步骤S1中脱胶的方法为:将蚕蛹毛油水浴加热到70℃,缓慢加入占油质量1%的磷酸,反应充分后,离心分别获得上层脱胶油。
4.根据权利要求2所述的一种链条润滑脂,其特征在于,所述步骤S1中脱酸的方法为:向脱胶蛹油中加入3 moL/L的NaOH溶液, 缓慢滴加并均匀搅拌加热到70 ℃保温30 min,冷却至室温,分离,提纯油相,得到精制蛹油。
5.如权利要求1所述的一种链条润滑脂的制备方法,其特征在于:将改性蚕蛹油基础油和矿物基础油混合均与后,加入脂肪酸锂皂在110-140℃进行炼制1-3h,再150-160℃下脱水1h,降温至80℃,加入剩余的成分,继续搅拌20-40min,研磨脱泡得到链条润滑脂。
6.根据权利要求5所述一种链条润滑脂的制备方法,其特征在于:所述矿物基础油为500SN矿物油。
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