CN116656412A - 一种多功能润滑脂及其制备方法 - Google Patents
一种多功能润滑脂及其制备方法 Download PDFInfo
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- CN116656412A CN116656412A CN202310604841.2A CN202310604841A CN116656412A CN 116656412 A CN116656412 A CN 116656412A CN 202310604841 A CN202310604841 A CN 202310604841A CN 116656412 A CN116656412 A CN 116656412A
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- multifunctional
- stirring
- lubricating grease
- silicone oil
- heating
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- 239000004519 grease Substances 0.000 title claims abstract description 53
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000003921 oil Substances 0.000 claims abstract description 34
- 229920013822 aminosilicone Polymers 0.000 claims abstract description 33
- 239000013538 functional additive Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000002199 base oil Substances 0.000 claims abstract description 25
- 239000002562 thickening agent Substances 0.000 claims abstract description 21
- BIGYLAKFCGVRAN-UHFFFAOYSA-N 1,3,4-thiadiazolidine-2,5-dithione Chemical compound S=C1NNC(=S)S1 BIGYLAKFCGVRAN-UHFFFAOYSA-N 0.000 claims abstract description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004327 boric acid Substances 0.000 claims abstract description 16
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 15
- 239000012459 cleaning agent Substances 0.000 claims abstract description 15
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 37
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 18
- 238000010992 reflux Methods 0.000 claims description 18
- 238000002390 rotary evaporation Methods 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 18
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- HASCQPSFPAKVEK-UHFFFAOYSA-N dimethyl(phenyl)phosphine Chemical compound CP(C)C1=CC=CC=C1 HASCQPSFPAKVEK-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- ORTVZLZNOYNASJ-UPHRSURJSA-N (z)-but-2-ene-1,4-diol Chemical compound OC\C=C/CO ORTVZLZNOYNASJ-UPHRSURJSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 239000002480 mineral oil Substances 0.000 claims description 5
- 235000010446 mineral oil Nutrition 0.000 claims description 5
- 239000000344 soap Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229920002367 Polyisobutene Polymers 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052796 boron Inorganic materials 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
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- 238000007599 discharging Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 4
- 230000001678 irradiating effect Effects 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- -1 butyl isooctyl dodecyl ammonium phosphate Chemical compound 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LJKQIQSBHFNMDV-UHFFFAOYSA-N 7-thiabicyclo[4.1.0]hepta-2,4-dien-6-ol Chemical compound C1=CC=CC2(O)C1S2 LJKQIQSBHFNMDV-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 241001633683 Centipeda <firmicute> Species 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000004443 Ricinus communis Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- RKKOMEIYHHASIN-UHFFFAOYSA-N hydroperoxyboronic acid Chemical compound OOB(O)O RKKOMEIYHHASIN-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/022—Boron compounds without C-boron linkages
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- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
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- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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- C10M2229/04—Siloxanes with specific structure
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Abstract
本发明涉及一种多功能润滑脂及其制备方法,属于润滑脂技术领域。该多功能润滑脂按照重量百分比计包括:稠化剂12‑18wt%、复合功能添加剂6.5‑9wt%、分散助剂0.9‑1.1wt%、洁净剂0.3‑0.5wt%、抗氧剂0.1‑0.2wt%,余量为基础油;其中,复合功能添加剂以二巯基噻二唑为原料,通过丁烯二醇点击反应引入支状羟基修饰,再与硼酸酯化,最后与氨基硅油作用,将含硼的硫氮杂环引入到氨基硅油的长链中,具有良好的热稳定性和耐热迁移性,制得的润滑脂具有优异的抗磨减磨效果。
Description
技术领域
本发明属于润滑脂技术领域,具体地,涉及一种多功能润滑脂及其制备方法。
背景技术
机械零部件在运转过程中会产生摩擦磨损,带来材料和能源的大量损耗,与此同时还会造成环境污染,一般具有相对运动的零部件之间均会填充润滑物质减轻摩擦;润滑脂是一种由基础油、稠化剂和添加剂构成的半流体状润滑材料,其技术水平与工业机械、交通运输和航空航天等各类高端装备制造业的发展密切相关,随着高端装备制造业的快速发展,越来越苛刻的工况对润滑脂节能、降耗和长寿命等指标不断提出更高的要求,不断对润滑脂进行高性能优化是润滑脂研究领域的重要发展趋势。
基础油是润滑脂的重要组成部分,约占润滑脂总重的75%-95%,基础油的结构和组成对润滑脂的关键性能和使役行为都有着显著的影响,其中,矿物油来源广、价格低、性能稳定而被广泛应用;稠化剂分散在基础油中并形成润滑脂的结构骨架,使基础油被吸附和固定在结构骨架中,现有技术中的稠化剂主要有皂基稠化剂和非皂基稠化剂两类;添加剂的主要作用是提高矿物油的特征性能,如极压抗磨、减磨、防锈、抗氧等性能,针对不同的服役工况,添加不同的添加剂;而对于提升润滑脂的极压抗磨性能的添加剂主要以磷系添加剂为主,其在摩擦面间可以形成磷酸盐润滑保护膜,从而达到抗磨减磨的作用,传统的润滑脂中以磷酸三甲酚酯类、丁基异辛基磷酸十二铵盐类添加剂应用最为广泛,但是,该类添加剂热稳定性不足,在摩擦面间存在局部高温,添加剂分解导致润滑膜失效,其次,耐热迁移性不足,该类添加剂绝大多数均为小分子化合物,在局部高温下易发生迁移,使得润滑膜的稳定性下降,特别是高转速、高载荷工况下,极易出现润滑失效,此外,磷系添加剂在摩擦过程中易产生污染物,造成环境污染。
发明内容
为了解决背景技术中提到的技术问题,本发明的目的在于提供一种多功能润滑脂及其制备方法。
本发明的目的可以通过以下技术方案实现:
一种多功能润滑脂,按照重量百分比计包括:稠化剂12-18wt%、复合功能添加剂6.5-9wt%、分散助剂0.9-1.1wt%、洁净剂0.3-0.5wt%、抗氧剂0.1-0.2wt%,余量为基础油;
所述复合功能添加剂由以下方法制备:
步骤A1:将二巯基噻二唑、二甲基苯基膦和乙醇溶液在氮气保护下搅拌溶解,再加入丁烯二醇,升温至70-80℃回流,施加200-300rpm机械搅拌和紫外辐照,反应2.5-3h,反应结束减压旋蒸脱除乙醇溶液,得到中间体1;
进一步地,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:30-40mg:800-900mL,乙醇溶液的质量分数为25-30%,紫外辐照强度400-500W/m2;在二甲基苯基膦和紫外辐照引发下,丁烯二醇中的双键和二巯基噻二唑中的巯基点击加成,引入支状羟基修饰。
步骤A2:将硼酸、对甲苯磺酸、二氧六环和去离子水搅拌溶解,再加入中间体1,施加120-180rpm机械搅拌,升温至90-100℃,回流反应4-5h,反应结束减压旋蒸脱除二氧六环和水分,得到中间体2;
进一步地,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:4.5-5.5g:100-150mL:180-240mL,以对甲苯磺酸为催化剂,促进硼酸与中间体1中引入的支状羟基酯化,引入有机硼结构。
步骤A3:将中间体2、氯化钯和四氢呋喃混合,升温至40-50℃,搅拌活化20-30min,再加入氨基硅油,施加600-700rpm机械搅拌,继续升温至65-75℃,回流反应3-4h,反应结束旋蒸脱除四氢呋喃,得到复合功能添加剂。
进一步地,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为20-30mg/kg,四氢呋喃的用量为氨基硅油质量的0.6-0.7倍,中间体2中的残余硼酸羟基与氨基硅油中的氨基反应,将中间体2接枝到硅链中。
进一步地,氨基硅油选自具有支链和端氨基型硅油。
一种多功能润滑脂的制备方法,具体操作为:将基础油和抗氧剂混合预升温至80-100℃,再加入稠化剂,升温至170-190℃,搅拌炼制6-8min,之后快速降温至120℃以下,加入复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨3-4次,得到多功能润滑脂。
进一步地,稠化剂为12-羟基硬脂酸锂皂。
进一步地,分散助剂为聚异丁烯PB2400。
进一步地,洁净剂为硫化烷基酚钙S206。
进一步地,抗氧剂为二烷基二硫代氨基甲酸锌T203。
进一步地,基础油为矿物油MV1500。
本发明的有益效果:
本发明在润滑脂中添加一种复合功能添加剂,提高润滑脂的极压抗磨、减磨性能,其由含硫氮杂环的二巯基噻二唑为原料,通过丁烯二醇点击反应引入支状羟基修饰,改善巯基的酯化能力,再与硼酸酯化,引入有机硼结构,硫氮杂环易与金属表面螯合,在摩擦过程中,将复合功能添加剂富集在金属表面,形成润滑膜,摩擦产生的局部高温促使形成氮硼类高强度化合物,强化润滑膜的强度,充分发挥润滑脂的减磨作用;且本发明采用丁烯二醇引入双支状羟基,提高硼元素与硫氮杂环的结合强度,避免摩擦产生的局部高温使得有机硼与硫氮杂环分解,从而导致硼元素无法在摩擦界面富集;此外,本发明中的硼酸还为桥接材料,将含硼的硫氮杂环引入到氨基硅油的长链中,利用硅氧链提高复合功能添加剂的热稳定性和耐水性,同时抗磨成分负载在大分子链中,提升耐热迁移性,达到稳定发挥减磨作用。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整的描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
为充分清楚地说明本发明的具体实施方法,将采用的原料公开如下:
基础油,选自矿物油,型号为MV1500,由中国石油化工股份有限公司荆门分公司提供;
稠化剂,选自12-羟基硬脂酸锂皂,由通辽市通华蓖麻化工有限责任公司提供;
分散助剂,选自低分子量聚异丁烯,型号为PB2400,由上海道普化学有限公司提供;
洁净剂,选自硫化烷基酚钙,型号为S206,由无锡南方石油添加剂有限公司提供;
抗氧剂,选自二烷基二硫代氨基甲酸锌,型号为T203,无锡南方石油添加剂有限公司;
氨基硅油,选自具有支链和端氨基型硅油,型号为KF-857,由苏州建道电子有限公司提供。
实施例1
本实施例多功能润滑脂,具体实施过程如下:
1)制备复合功能添加剂
1.1、配制质量分数为30%的乙醇溶液,取二巯基噻二唑、二甲基苯基膦和乙醇溶液投加到充满氮气的反应器中,施加机械搅拌溶解,再投加丁烯二醇混合,升温至80℃回流,控制搅拌速率为300rpm,采用紫外灯辐照,控制辐照强度为500W/m2,控制反应时间为2.5h,反应中,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:40mg:900mL,反应结束减压旋蒸脱除乙醇溶液,即制得中间体1。
1.2、取将硼酸、对甲苯磺酸、二氧六环和去离子水投加到反应器中,施加机械搅拌溶解,再投加中间体1,施加180rpm机械搅拌,升温至100℃,回流反应4h,反应中,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:5.5g:150mL:180mL,反应结束减压旋蒸脱除二氧六环和水分,即制得中间体2。
1.3、取中间体2、氯化钯和四氢呋喃投料混合,升温至50℃,辅以120rpm搅拌活化20min,再加入氨基硅油,提升搅拌速率为700rpm,继续升温至75℃,回流反应3h,反应中,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为30mg/kg,四氢呋喃的用量为氨基硅油质量的0.7倍,反应结束旋蒸脱除四氢呋喃,即制得复合功能添加剂。
2)制备多功能润滑脂
2.1、按照重量百分比计取:基础油79.8wt%、稠化剂12wt%、复合功能添加剂6.5wt%、分散助剂1.0wt%、洁净剂0.5wt%和抗氧剂0.2wt%。
2.2、将基础油和抗氧剂混合投加到电子调温电热套中,预升温至100℃,再投加稠化剂,施加80rpm搅拌,升温至190℃炼制6min,采用冷却水快速降温至不高于120℃,投加复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨3次,出料即制得多功能润滑脂。
实施例2
本实施例多功能润滑脂,具体实施过程如下:
1)制备复合功能添加剂
1.1、配制质量分数为25%的乙醇溶液,取二巯基噻二唑、二甲基苯基膦和乙醇溶液投加到充满氮气的反应器中,施加机械搅拌溶解,再投加丁烯二醇混合,升温至70℃回流,控制搅拌速率为200rpm,采用紫外灯辐照,控制辐照强度为400W/m2,控制反应时间为3h,反应中,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:30mg:800mL,反应结束减压旋蒸脱除乙醇溶液,即制得中间体1。
1.2、取将硼酸、对甲苯磺酸、二氧六环和去离子水投加到反应器中,施加机械搅拌溶解,再投加中间体1,施加120rpm机械搅拌,升温至90℃,回流反应5h,反应中,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:4.5g:100mL:240mL,反应结束减压旋蒸脱除二氧六环和水分,即制得中间体2。
1.3、取中间体2、氯化钯和四氢呋喃投料混合,升温至40℃,辅以120rpm搅拌活化30min,再加入氨基硅油,提升搅拌速率为600rpm,继续升温至65℃,回流反应4h,反应中,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为20mg/kg,四氢呋喃的用量为氨基硅油质量的0.6倍,反应结束旋蒸脱除四氢呋喃,即制得复合功能添加剂。
2)制备多功能润滑脂
2.1、按照重量百分比计取:基础油73.4wt%、稠化剂16wt%、复合功能添加剂9wt%、分散助剂1.1wt%、洁净剂0.4wt%和抗氧剂0.1wt%。
2.2、将基础油和抗氧剂混合投加到电子调温电热套中,预升温至80℃,再投加稠化剂,施加80rpm搅拌,升温至170℃炼制8min,采用冷却水快速降温至不高于120℃,投加复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨4次,出料即制得多功能润滑脂。
实施例3
本实施例多功能润滑脂,具体实施过程如下:
1)制备复合功能添加剂
1.1、配制质量分数为25%的乙醇溶液,取二巯基噻二唑、二甲基苯基膦和乙醇溶液投加到充满氮气的反应器中,施加机械搅拌溶解,再投加丁烯二醇混合,升温至75℃回流,控制搅拌速率为300rpm,采用紫外灯辐照,控制辐照强度为500W/m2,控制反应时间为2.8h,反应中,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:35mg:900mL,反应结束减压旋蒸脱除乙醇溶液,即制得中间体1。
1.2、取将硼酸、对甲苯磺酸、二氧六环和去离子水投加到反应器中,施加机械搅拌溶解,再投加中间体1,施加180rpm机械搅拌,升温至100℃,回流反应4h,反应中,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:5g:120mL:200mL,反应结束减压旋蒸脱除二氧六环和水分,即制得中间体2。
1.3、取中间体2、氯化钯和四氢呋喃投料混合,升温至50℃,辅以120rpm搅拌活化30min,再加入氨基硅油,提升搅拌速率为700rpm,继续升温至70℃,回流反应4h,反应中,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为20mg/kg,四氢呋喃的用量为氨基硅油质量的0.7倍,反应结束旋蒸脱除四氢呋喃,即制得复合功能添加剂。
2)制备多功能润滑脂
2.1、按照重量百分比计取:基础油74.9wt%、稠化剂15wt%、复合功能添加剂8.5wt%、分散助剂1.1wt%、洁净剂0.4wt%和抗氧剂0.1wt%。
2.2、将基础油和抗氧剂混合投加到电子调温电热套中,预升温至90℃,再投加稠化剂,施加80rpm搅拌,升温至180℃炼制8min,采用冷却水快速降温至不高于120℃,投加复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨4次,出料即制得多功能润滑脂。
实施例4
本实施例多功能润滑脂,具体实施过程如下:
1)制备复合功能添加剂
1.1、配制质量分数为25%的乙醇溶液,取二巯基噻二唑、二甲基苯基膦和乙醇溶液投加到充满氮气的反应器中,施加机械搅拌溶解,再投加丁烯二醇混合,升温至80℃回流,控制搅拌速率为300rpm,采用紫外灯辐照,控制辐照强度为400W/m2,控制反应时间为3h,反应中,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:30mg:900mL,反应结束减压旋蒸脱除乙醇溶液,即制得中间体1。
1.2、取将硼酸、对甲苯磺酸、二氧六环和去离子水投加到反应器中,施加机械搅拌溶解,再投加中间体1,施加180rpm机械搅拌,升温至90℃,回流反应5h,反应中,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:5.5g:150mL:220mL,反应结束减压旋蒸脱除二氧六环和水分,即制得中间体2。
1.3、取中间体2、氯化钯和四氢呋喃投料混合,升温至45℃,辅以120rpm搅拌活化20min,再加入氨基硅油,提升搅拌速率为600rpm,继续升温至75℃,回流反应4h,反应中,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为25mg/kg,四氢呋喃的用量为氨基硅油质量的0.6倍,反应结束旋蒸脱除四氢呋喃,即制得复合功能添加剂。
2)制备多功能润滑脂
2.1、按照重量百分比计取:基础油72.9wt%、稠化剂18wt%、复合功能添加剂7.8wt%、分散助剂0.9wt%、洁净剂0.3wt%和抗氧剂0.1wt%。
2.2、将基础油和抗氧剂混合投加到电子调温电热套中,预升温至100℃,再投加稠化剂,施加80rpm搅拌,升温至180℃炼制8min,采用冷却水快速降温至不高于120℃,投加复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨4次,出料即制得多功能润滑脂。
对比例
本对比例与实施例3的制备过程相同,将复合功能添加剂替换为现有的极压抗磨剂,由磷酸三甲酚酯极压抗磨剂T306和丁基异辛基磷酸十二铵盐极压抗磨剂T308按照质量比为2:1混合而成,用量为5.8wt%。
取实施例1-实施例4以及对比例制备的润滑脂,对润滑脂的基础理化性能测试,具体如表1所示:
表1
由表1数据可知,本发明制备的润滑脂理化性能良好,符合润滑脂的一般技术指标要求,其中,从数据中可以看出,本发明制备的润滑脂相较于对比例,滴点较高,蒸发损失量较低,具有高温稳定特点,水淋流失量明显低于对比例,表现出良好的耐水性。
基于以上测试数据,取实施例1-实施例4制备的复合功能添加剂,对比例复配的极压抗磨剂,以及基础油,采用SDTQ600型同步热分析仪进行热稳定性测试,测试氛围为氮气,升温速率为10℃/min,以热重损失达到5%作为开始分解温度,具体测试数据如表2所示:
表2
由表2数据可知,基础油的开始分解温度约为215℃,本发明制备的复合功能添加剂开始分解温度为198-210℃,与基础油相近,可在较高温度下与基础油共同发挥润滑作用。
取实施例1-实施例4以及对比例制备的润滑脂,采用MRS-12DA型极压四球试验机测试最大无卡咬负荷(PB)、烧结负荷(PD)、磨斑直径和摩擦因数,长磨试验温度为100℃,时间为60min,压力为294N,速率为450r/min,具体测试数据如表3所示:
表3
由表3数据可知,本发明制备的润滑脂最大无卡咬负荷和烧结负荷均明显大于对比例,具有良好的极压润滑性,磨斑直径和平均摩擦因数均低于对比例,表现出良好减磨作用。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (9)
1.一种多功能润滑脂,其特征在于,按照重量百分比计包括:稠化剂12-18wt%、复合功能添加剂6.5-9wt%、分散助剂0.9-1.1wt%、洁净剂0.3-0.5wt%、抗氧剂0.1-0.2wt%,余量为基础油;
所述复合功能添加剂由以下方法制备:
步骤A1:将二巯基噻二唑、二甲基苯基膦和乙醇溶液在氮气保护下搅拌溶解,再加入丁烯二醇,升温至70-80℃回流,搅拌并辅以紫外辐照反应2.5-3h,反应结束减压旋蒸脱除乙醇溶液,得到中间体1;
步骤A2:将硼酸、对甲苯磺酸、二氧六环和去离子水搅拌溶解,再加入中间体1,搅拌并升温至90-100℃,回流反应4-5h,反应结束减压旋蒸脱除二氧六环和水分,得到中间体2;
步骤A3:将中间体2、氯化钯和四氢呋喃混合,升温至40-50℃,搅拌活化20-30min,再加入氨基硅油,搅拌并继续升温至65-75℃,回流反应3-4h,反应结束旋蒸脱除四氢呋喃,得到复合功能添加剂。
2.根据权利要求1所述的一种多功能润滑脂,其特征在于,二巯基噻二唑、丁烯二醇、二甲基苯基膦和乙醇溶液的用量比为0.1mol:0.2mol:30-40mg:800-900mL,乙醇溶液的质量分数为25-30%。
3.根据权利要求2所述的一种多功能润滑脂,其特征在于,中间体1、硼酸、对甲苯磺酸、二氧六环和去离子水的用量比为0.1mol:0.1mol:4.5-5.5g:100-150mL:180-240mL。
4.根据权利要求3所述的一种多功能润滑脂,其特征在于,氨基硅油的氨基含量与中间体2的摩尔比为1:1,氯化钯与氨基硅油和中间体2总量比为20-30mg/kg,四氢呋喃的用量为氨基硅油质量的0.6-0.7倍。
5.根据权利要求4所述的一种多功能润滑脂,其特征在于,氨基硅油为具有支链和端氨基型硅油。
6.根据权利要求5所述的一种多功能润滑脂的制备方法,其特征在于,具体操作为:将基础油和抗氧剂混合预升温至80-100℃,再加入稠化剂,升温至170-190℃,搅拌炼制6-8min,之后快速降温至120℃以下,加入复合功能添加剂、分散助剂和洁净剂,采用三辊研磨机研磨3-4次,得到多功能润滑脂。
7.根据权利要求6所述的一种多功能润滑脂的制备方法,其特征在于,基础油为矿物油MV1500。
8.根据权利要求6所述的一种多功能润滑脂的制备方法,其特征在于,稠化剂为12-羟基硬脂酸锂皂。
9.根据权利要求6所述的一种多功能润滑脂的制备方法,其特征在于,分散助剂为聚异丁烯PB2400。
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