CN106590858A - 一种耐高温自锁螺母用二硫化钼干膜润滑剂及其制作方法 - Google Patents
一种耐高温自锁螺母用二硫化钼干膜润滑剂及其制作方法 Download PDFInfo
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- CN106590858A CN106590858A CN201610918245.1A CN201610918245A CN106590858A CN 106590858 A CN106590858 A CN 106590858A CN 201610918245 A CN201610918245 A CN 201610918245A CN 106590858 A CN106590858 A CN 106590858A
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- epoxy resin
- locking nut
- molybdenum bisuphide
- lubricating agent
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- 239000000314 lubricant Substances 0.000 title claims abstract description 28
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title abstract 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title abstract 3
- 238000002360 preparation method Methods 0.000 title description 5
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 20
- 239000003822 epoxy resin Substances 0.000 claims abstract description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 239000004642 Polyimide Substances 0.000 claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims abstract description 7
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000013081 microcrystal Substances 0.000 claims abstract description 7
- 239000012188 paraffin wax Substances 0.000 claims abstract description 7
- 229920001721 polyimide Polymers 0.000 claims abstract description 7
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims abstract description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 28
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 27
- 239000011733 molybdenum Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 abstract 2
- 239000004698 Polyethylene Substances 0.000 abstract 1
- 239000010426 asphalt Substances 0.000 abstract 1
- 229910000397 disodium phosphate Inorganic materials 0.000 abstract 1
- 235000019800 disodium phosphate Nutrition 0.000 abstract 1
- 239000004519 grease Substances 0.000 abstract 1
- -1 polyethylene Polymers 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- 239000001993 wax Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 4
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- 238000012360 testing method Methods 0.000 description 4
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- 239000004593 Epoxy Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
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- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007866 anti-wear additive Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000005764 inhibitory process 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- ZMQBAPPSYGILGT-UHFFFAOYSA-N sodium;2,3-bis(hydroxymethyl)butanedioic acid Chemical compound [Na+].OCC(C(O)=O)C(CO)C(O)=O ZMQBAPPSYGILGT-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
Classifications
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- 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
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
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- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C10M2201/066—Molybdenum sulfide
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- C10M2201/085—Phosphorus oxides, acids or salts
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Abstract
本发明公开了一种耐高温自锁螺母用二硫化钼干膜润滑剂，由下列重量份的原料制成：601环氧树脂90‑91、618环氧树脂31‑32、聚酰亚胺5‑8、聚乙烯蜡4‑6、二硫化钼24‑27、三氧化二锑12‑14、甲基六氢苯酐3.7‑3.9、二茂铁1.5‑1.9、石蜡乳液2‑3、纳米碳酸钙4.4‑4.8、甲基三乙氧基硅烷0.2‑0.4、磷酸氢二钠0.1‑0.3、微晶粉6‑7、沥青2.1‑2.5、混合溶剂60‑62，利用本发明制得的干膜润滑剂与常规油脂润滑比较，具有成本低、耐热温度高、使用范围广等优点。
Description
技术领域
本发明涉及润滑剂制备技术领域，尤其涉及一种耐高温自锁螺母用二硫化钼干膜润滑剂及其制作方法。
背景技术
自锁螺母除具有普通螺母的紧固作用以外，还具有锁紧性能，其工作原理一般是靠摩擦力自锁，可以防止在使用中紧固元件发生松动、脱落现象，广泛应用于航空、航天飞行器等机械活动部件的紧固。微动磨损在工业领域普遍存在，被称为工业中的＂癌症＂，自锁螺母在装配或使用过程中不仅由于各种各样的振动环境极易发生微动磨损损伤，而且因多次拧入、拧出经常与发生基体金属相互摩擦、粘接的现象，从而导致螺母的锁紧性能失效，进而对整体机械的结构产生影响，降低了机械的可靠性以及使用寿命，喷涂润滑剂是降低摩擦和减少磨损的有效途径之一。
干膜润滑剂是一种将固体润滑剂、耐磨添加剂等分散于有机或无机粘结剂体系中，通过喷涂、刷涂、浸涂等工艺在摩擦部件表面上成膜以降低其摩擦与磨损的一种新型润滑技术，尤其是有机粘结干膜润滑剂，使用简单，施工方便，将其应用于自锁螺母可在高低温、高负荷、超高真空、强氧化还原和强辐射等环境下有效地润滑，是目前品种最多、应用最广的一类干膜润滑剂。例如《航空航天用热固性二硫化钼干膜润滑剂的研制》一文采用酸酐、601和618混合环氧树脂、胶体二硫化钼及特殊溶剂和添加剂等制备成的热固性二硫化钼干膜润滑剂，结果表明，其膜层不仅附着力、防腐性、耐高低温性及耐液体介质性好，而且在热真空环境下工作性能稳定、摩擦系数低、耐磨寿命长。
但是，目前使用的二硫化钼干膜的突出缺点是在大气(特别在潮湿大气)中容易氧化而发生润滑失效。真空中二硫化钼在1100℃时分解成Mo和S；在空气中，当温度超过400℃时，产生明显的氧化，并生成三氧化钼，影响其润滑性及其对金属表面的粘附作用，因此在空气中二硫化钼可用至350℃，温度再高时摩擦磨损都会增大，为此需要提高干膜的耐潮湿性及耐高温性能，此外，文献中制得的干膜润滑剂使用的环氧树脂粘接剂耐温性能较差，也是导致干膜润滑剂耐温性能相对较差的原因之一，而且文中的干膜润滑剂结构功能都较为单一，仅仅具有润滑作用，涂覆在自锁螺母表面起不到防锈作用，且承载力低、防腐蚀性差、不易去除。
发明内容
本发明目的就是为了弥补已有技术的缺陷，提供一种耐高温自锁螺母用二硫化钼干膜润滑剂及其制作方法。
本发明是通过以下技术方案实现的：
一种耐高温自锁螺母用二硫化钼干膜润滑剂，由下列重量份的原料制成：601环氧树脂90-91、618环氧树脂31-32、聚酰亚胺5-8、聚乙烯蜡4-6、二硫化钼24-27、三氧化二锑12-14、甲基六氢苯酐3.7-3.9、二茂铁1.5-1.9、石蜡乳液2-3、纳米碳酸钙4.4-4.8、甲基三乙氧基硅烷0.2-0.4、磷酸氢二钠0.1-0.3、微晶粉6-7、沥青2.1-2.5、混合溶剂60-62，所述的混合溶剂是由乙二醇单乙醚、二甲苯与丙酮按照质量百分比1∶5∶4混合而成。
所述的一种耐高温自锁螺母用二硫化钼干膜润滑剂的制作方法，包括以下步骤：
（1）将微晶粉在干燥箱中100-120℃预热干燥1-2小时，加入质量分数为5-8%的磷酸氢二钠溶液，在60-90℃下超声研磨20-30分钟，喷雾干燥，于1000-1100℃温度下煅烧15-20分钟，冷却至室温加入二茂铁研磨20-30分钟得改性微晶粉；
（2）将纳米碳酸钙在干燥箱中100-120℃预热干燥1-2小时，保持温度加入甲基三乙氧基硅烷搅拌10-15分钟，真空干燥得改性纳米碳酸钙；
（3）将601环氧树脂、618环氧树脂、聚酰亚胺投入高混机中加入混合溶剂升温至85-95℃搅拌至全部溶解，加入步骤（2）物料、聚乙烯蜡高速搅拌20-30分钟得无机纳米改性的混合环氧树脂液；
（4）将二硫化钼、三氧化二锑于750-850℃煅烧处理30-40分钟，降温至110-120℃加入石蜡乳液、步骤（1）物料研磨1-2小时，于75-85℃加入步骤（3）物料及其他剩余成分超声分散研磨2-4小时，出料。
本发明的优点是：本发明以二硫化钼为润滑剂，二硫化钼中S原子暴露在二硫化钼晶体层的表面, 与金属表面原子形成化学键从而对金属表面产生很强的粘附作用,易形成转移膜,在各种摩擦条件下, 二硫化钼在金属上的转移膜呈明显的取向排列,其基础面平行于金属表面,因此降低了摩擦磨损，在摩擦过程中,添加的三氧化二锑不仅起到了承载的作用可以使二硫化钼更好的取向，与二硫化钼协同抗磨，还提高产品的耐高温性能和硬度；将601环氧树脂、618环氧树脂进行复合无机纳米改性后作为有机粘结剂，改善了粘结剂的耐高温性能和耐候性，最后再配伍改性的微晶粉作为填料及其他有效添加剂，明显改善了干膜润滑剂的润滑性和防锈耐潮性能，制得的干膜润滑剂与常规油脂润滑比较，具有成本低、耐热温度高、使用范围广等优点。
具体实施方式
一种耐高温自锁螺母用二硫化钼干膜润滑剂，由下列重量份的原料制成：601环氧树脂90、618环氧树脂31、聚酰亚胺5、聚乙烯蜡4、二硫化钼24、三氧化二锑12、甲基六氢苯酐3.7、二茂铁1.5、石蜡乳液2、纳米碳酸钙4.4、甲基三乙氧基硅烷0.2、磷酸氢二钠0.1、微晶粉6、沥青2.1、混合溶剂60，所述的混合溶剂是由乙二醇单乙醚、二甲苯与丙酮按照质量百分比1∶5∶4混合而成。
所述的一种耐高温自锁螺母用二硫化钼干膜润滑剂的制作方法，包括以下步骤：
（1）将微晶粉在干燥箱中100-120℃预热干燥1-2小时，加入质量分数为5-8%的磷酸氢二钠溶液，在60-90℃下超声研磨20-30分钟，喷雾干燥，于1000-1100℃温度下煅烧15-20分钟，冷却至室温加入二茂铁研磨20-30分钟得改性微晶粉；
（2）将纳米碳酸钙在干燥箱中100-120℃预热干燥1-2小时，保持温度加入甲基三乙氧基硅烷搅拌10-15分钟，真空干燥得改性纳米碳酸钙；
（3）将601环氧树脂、618环氧树脂、聚酰亚胺投入高混机中加入混合溶剂升温至85-95℃搅拌至全部溶解，加入步骤（2）物料、聚乙烯蜡高速搅拌20-30分钟得无机纳米改性的混合环氧树脂液；
（4）将二硫化钼、三氧化二锑于750-850℃煅烧处理30-40分钟，降温至110-120℃加入石蜡乳液、步骤（1）物料研磨1-2小时，于75-85℃加入步骤（3）物料及其他剩余成分超声分散研磨2-4小时，出料。
利用本发明制得的干膜润滑剂具有如下技术指标：
（1）将试片400℃下保温10min，取出在室温下保持10min为一循环，共进行10循试验，观察涂层表面未发现裂纹、变软等现象，耐高温性和耐温度交变性能良好；
（2）将试片分别在70℃的RP-3燃油和120℃的HH-2航空滑油中浸泡100h，观察涂层表面，未发现起泡、变软和脱落等现象，耐油性良好；
（3）按照HB6688—1992试验其承载能力为8550N，耐磨寿命（4450N）为250min；
（4）按照ASTM D2625试验其摩擦系数为：0.045。
Claims (2)
1.一种耐高温自锁螺母用二硫化钼干膜润滑剂，其特征在于，由下列重量份的原料制成：601环氧树脂90-91、618环氧树脂31-32、聚酰亚胺5-8、聚乙烯蜡4-6、二硫化钼24-27、三氧化二锑12-14、甲基六氢苯酐3.7-3.9、二茂铁1.5-1.9、石蜡乳液2-3、纳米碳酸钙4.4-4.8、甲基三乙氧基硅烷0.2-0.4、磷酸氢二钠0.1-0.3、微晶粉6-7、沥青2.1-2.5、混合溶剂60-62，所述的混合溶剂是由乙二醇单乙醚、二甲苯与丙酮按照质量百分比1∶5∶4混合而成。
2.根据权利要求1所述的一种耐高温自锁螺母用二硫化钼干膜润滑剂的制作方法，其特征在于包括以下步骤：
（1）将微晶粉在干燥箱中100-120℃预热干燥1-2小时，加入质量分数为5-8%的磷酸氢二钠溶液，在60-90℃下超声研磨20-30分钟，喷雾干燥，于1000-1100℃温度下煅烧15-20分钟，冷却至室温加入二茂铁研磨20-30分钟得改性微晶粉；
（2）将纳米碳酸钙在干燥箱中100-120℃预热干燥1-2小时，保持温度加入甲基三乙氧基硅烷搅拌10-15分钟，真空干燥得改性纳米碳酸钙；
（3）将601环氧树脂、618环氧树脂、聚酰亚胺投入高混机中加入混合溶剂升温至85-95℃搅拌至全部溶解，加入步骤（2）物料、聚乙烯蜡高速搅拌20-30分钟得无机纳米改性的混合环氧树脂液；
（4）将二硫化钼、三氧化二锑于750-850℃煅烧处理30-40分钟，降温至110-120℃加入石蜡乳液、步骤（1）物料研磨1-2小时，于75-85℃加入步骤（3）物料及其他剩余成分超声分散研磨2-4小时，出料。
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| 朱廷彬: "《润滑脂技术大全》", 29 April 2005, 《中国石化出版社》 * |
| 桂立丰 等: "《机械工程材料测试手册》", 31 May 2002, 辽宁科学技术出版社 * |
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