CN109097158A - 一种添加改性石墨烯的机器人谐波减速器润滑脂组合物及其制备方法 - Google Patents
一种添加改性石墨烯的机器人谐波减速器润滑脂组合物及其制备方法 Download PDFInfo
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- CN109097158A CN109097158A CN201810922571.9A CN201810922571A CN109097158A CN 109097158 A CN109097158 A CN 109097158A CN 201810922571 A CN201810922571 A CN 201810922571A CN 109097158 A CN109097158 A CN 109097158A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 19
- 239000000314 lubricant Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004519 grease Substances 0.000 claims abstract description 60
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 230000001050 lubricating effect Effects 0.000 claims abstract description 40
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000007822 coupling agent Substances 0.000 claims description 20
- 239000002585 base Substances 0.000 claims description 19
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 11
- 208000005156 Dehydration Diseases 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
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- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- 239000002199 base oil Substances 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 238000010008 shearing Methods 0.000 claims description 8
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
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- 229930195729 fatty acid Natural products 0.000 claims description 5
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
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- 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
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 229910003978 SiClx Inorganic materials 0.000 claims 1
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- 229910052791 calcium Inorganic materials 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims 1
- 229910021389 graphene Inorganic materials 0.000 abstract description 27
- 238000005461 lubrication Methods 0.000 abstract description 7
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 12
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 10
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 5
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- 229940114072 12-hydroxystearic acid Drugs 0.000 description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 4
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- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- KIHBGTRZFAVZRV-UHFFFAOYSA-N 2-Hydroxyoctadecanoic acid Natural products CCCCCCCCCCCCCCCCC(O)C(O)=O KIHBGTRZFAVZRV-UHFFFAOYSA-N 0.000 description 3
- 241000446313 Lamella Species 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- SXNBVULTHKFMNO-UHFFFAOYSA-N 2,2-dihydroxyoctadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)(O)C(O)=O SXNBVULTHKFMNO-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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Abstract
本发明公开了一种添加改性石墨烯的机器人谐波减速器润滑脂组合物及其制备方法。所述润滑脂组合物包括润滑脂和占润滑脂重量0.001～0.2%的掺杂二氧化硅的改性石墨烯。所述润滑脂组合物不仅利用石墨烯超硬、超润滑、导热性好的特性，还有二氧化硅粉末的良好导热性，与已有的添加石墨烯润滑脂相比，该添加改性石墨烯润滑脂更具有良好的使用寿命，具有极低的摩擦系数（摩擦系数小于0.1）和优良的散热性能（热传导系数大于2.5 W/mK），具有较大的应用前景。
Description
技术领域
本发明涉及润滑脂技术领域，更具体地，涉及一种添加改性石墨烯的机器人谐波减速器润滑脂组合物及其制备方法。
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。根据用途可分为通用润滑脂和专用润滑脂两种，前者用于一般机械零件，后者用于拖拉机、铁道机车、船舶机械、石油钻井机械、阀门等。
随着电子行业、汽车行业和精密机械行业在中国的迅速发展，在高度洁净环境下的精密自动化生产线的应用越来越广泛。为了减少人工、提高生产效率和提高生产质量稳定性，这些生产线上应用了大量的精密工业机器人，其中精密工业机器人谐波减速器使用的润滑脂，要求摩擦系数低而稳定，导热系数高，润滑寿命长。近年来，世界机器人产业持续发展壮大，特种机器人特别是服务机器人作为新兴产业发展迅猛，我国目前机器人使用密度仍远低于世界平均水平。目前，韩国和日本是世界机器人使用密度最高的国家，每万名工人中拥有机器人数量超过300台，德国和美国超过250台，世界平均水平为58台，而我国仅为23台，因此我国机器人市场还有很大的增长空间。
石墨烯是2004年由英国科学家Novoselow等首次发现的，是由碳原子紧密堆积而成的新型二维原子晶体，其基本结构为sp2杂化碳原子形成的类六元环苯单元，是目前世界上最薄的二维材料，单层厚度只有0.3354nm。石墨烯上具有独特的热性能和力学性能，石墨烯的理论热导率达5000W/(m·K)，其机械强度可达130Ga。石墨烯这些独特性能，使其已成为近年来备受瞩目的国际前沿和研究热点，并展现出广阔的应用前景。但是任何方法所合成出来的石墨烯都易发生团聚效应进而影响其实际应用。
根据工业机器人谐波减速器的工况特点，要求润滑脂具有良好的稳定性能，润滑脂长时间使用不发生漏油、氧化；工业机器人谐波减速器需频繁启停且经常往复运动，易产生微动磨损，要求润滑脂具有优异的抗微动磨损性能；具有优异的极压抗磨性能；工业机器人谐波减速器上承受的转矩大，容易产生磨损，因此要求润滑脂具有优异的极压抗磨性能；具有良好的散热性能，在较低温度下仍可以正常启动和运转。
目前还尚未有添加石墨烯的工业机器人谐波减速器润滑脂的相关研究或报道。
发明内容
本发明所要解决的技术问题是克服现有石墨烯以及工业机器人谐波减速器润滑脂研究存在的缺陷和不足，提供一种改性石墨烯以及添加有该改性石墨烯的业机器人谐波减速器润滑脂。
本发明的第一个目的是提供一种掺杂二氧化硅的改性石墨烯。
本发明的第二个目的是提供一种添加改性石墨烯的机器人谐波减速器润滑脂组合物。
本发明的第三个目的是提供所述添加改性石墨烯的机器人谐波减速器润滑脂组合物的制备方法。
本发明的上述目的是通过以下技术方案给予实现的：
一种掺杂二氧化硅的改性石墨烯的制备方法，将过量石墨烯粉末分散在水中，剧烈搅拌，得到均匀分散液；然后将正硅酸乙酯，十六烷基三甲基溴化铵加入到上述溶液中，搅拌10～50分钟后将混合物于150～250℃水热处理2～4小时，分离沉淀、洗净、干燥，制得掺杂二氧化硅的改性石墨烯。
本发明采用化合物掺杂法，根据静电吸附的原理，二氧化硅可以沿石墨稀的两面定向生长，制成一种“三明治”结构或其它独特结构的石墨稀/二氧化硅复合纳米材料。该材料的优势在于：(1)利用二氧化硅的应力作用，所制复合材料为二维结构且独立分散，不易发生纳米团聚；(2)在充分发挥二氧化硅介孔结构特性和良好的导热性的同时，可以利用石墨稀超硬、超润滑、导热性好的性能，拓展了石墨烯在润滑脂方面的应用。
优选地，所述石墨烯、正硅酸乙酯与十六烷基三甲基溴化铵的质量比为1～3:20～80:100。
同时，本发明还请求保护上述制备方法制备得到的掺杂二氧化硅的改性石墨烯。
本发明制备得到的掺杂二氧化硅的改性石墨烯具有石墨烯超硬、超润滑、导热性好的特性，还有二氧化硅粉末的良好导热性，拓展了其在润滑脂方面的应用。因此，所述掺杂二氧化硅的改性石墨烯在制备润滑脂，尤其是在制备机器人谐波减速器润滑脂中的应用也在本发明保护范围内。
一种添加改性石墨烯的机器人谐波减速器润滑脂组合物，包括润滑脂和占润滑脂重量0.001～0.2％(优选为0.001～0.005％)的掺杂二氧化硅的改性石墨烯。
优选地，所述润滑脂为锂基润滑脂、钙基润滑脂、钠基润滑脂、铝基润滑脂、极压润滑脂或硅酸润滑脂。
优选地，所述掺杂二氧化硅的改性石墨烯还需经表面改性偶联剂改性。
本发明还请求保护一种新型抗磨剂，是将掺杂二氧化硅的改性石墨烯再经过改性偶联剂改性制备得到。
优选地，所述表面改性偶联剂为硬脂酸、油酸、γ-缩水甘油氧基丙基三甲氧基硅烷和十六烷基三甲基溴化铵中的一种或几种。
优选地，所述表面改性偶联剂为掺杂二氧化硅的改性石墨烯的重量含量的0.1～2％(优选为0.1～1％)。
所述的新型抗磨剂在制备机器人谐波减速器润滑脂中的应用也在本发明保护范围内。
一种添加改性石墨烯的机器人谐波减速器润滑脂组合物的制备方法，包括如下步骤：
S1.将掺杂二氧化硅的改性石墨烯添加到含有表面改性偶联剂改性的溶剂中，超声乳化后30℃～60℃处理3～6h，过滤、干燥后制得改性石墨烯粉体；
S2.将基础油预热，然后加入脂肪酸、碱以及0.001～0.2％S1制得改性石墨烯粉体，100～115℃皂化3小时后升温至200～210℃脱水，急冷至温度145～165℃，然后剪切、均质和脱气，制得润滑脂组合物；
其中，S1所述表面改性偶联剂的含量为掺杂二氧化硅的改性石墨烯的重量的0.1～2％。
优选地，基础油用量为84～99％、脂肪酸为0.1～15％、碱为0.1～15％。
优选地，所述表面改性偶联剂为硬脂酸、油酸、γ-缩水甘油氧基丙基三甲氧基硅烷和十六烷基三甲基溴化铵中的一种或几种。
优选地，所述脂肪酸为硬脂酸、12-羟基硬脂酸或羟硬脂酸。
优选地，所述碱为氢氧化锂、氢氧化钙或氢氧化钠。
与现有技术相比，本发明具有以下有益效果：
(1)本发明得到的掺杂二氧化硅的改性石墨烯利用二氧化硅的应力作用，所制复合材料为二维结构且独立分散，不易发生纳米团聚。
(2)本发明添加改性石墨烯的机器人谐波减速器润滑脂组合物，不仅利用石墨烯超硬、超润滑、导热性好特性的特性，还有二氧化硅粉末的良好导热性，通过具有抗磨性能的表面改性，制备出性能优异的新型抗磨剂。与已有的添加石墨烯润滑脂相比，该添加改性石墨烯润滑脂更具有良好的使用寿命，具有极低的摩擦系数(摩擦系数小于0.1)和优良的散热性能(热传导系数大于2.5W/mK)。
具体实施方式
以下结合具体实施例来进一步说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明，以下实施例所用试剂和材料均为市购。
实施例1
将30mg石墨烯(过量)分散在去离子水中，剧烈搅拌，得到均匀的分散液。然后将0.75g正硅酸乙酯，1.0g十六烷基三甲基溴化铵加入到上述溶液中。搅拌30分钟后，将混合物转移到聚四氟乙烯内衬不锈钢高压釜中，在200℃水热处理3小时。石墨稀片层上的周围并发生水解，形成溶胶。高压釜冷却至室温后，用吸滤分离法分离沉淀。用蒸馏水洗净，在60℃真空下充分干燥，即可得到掺杂二氧化硅的改性石墨烯。
实施例2
将10mg石墨烯(过量)分散在去离子水中，剧烈搅拌，得到均匀的分散液。然后将0.50g正硅酸乙酯，1.0g十六烷基三甲基溴化铵加入到上述溶液中。搅拌10分钟后，将混合物转移到聚四氟乙烯内衬不锈钢高压釜中，在250℃水热处理2小时。石墨稀片层上的周围并发生水解，形成溶胶。高压釜冷却至室温后，用吸滤分离法分离沉淀。用蒸馏水洗净，在60℃真空下充分干燥，即可得到掺杂二氧化硅的改性石墨烯。
实施例3
将20mg石墨烯(过量)分散在去离子水中，剧烈搅拌，得到均匀的分散液。然后将0.22g正硅酸乙酯，1.0g十六烷基三甲基溴化铵加入到上述溶液中。搅拌50分钟后，将混合物转移到聚四氟乙烯内衬不锈钢高压釜中，在150℃水热处理4小时。石墨稀片层上的周围并发生水解，形成溶胶。高压釜冷却至室温后，用吸滤分离法分离沉淀。用蒸馏水洗净，在60℃真空下充分干燥，即可得到掺杂二氧化硅的改性石墨烯。
实施例4
将实施例1得到的改性石墨烯，加入1g到含有0.01g油酸表面改性偶联剂的溶剂，通过超声分乳化后在温度为30℃处理6h，过滤、干燥后制得改性石墨烯粉体；将90g润滑脂的基础油预热，然后加入5g硬脂酸，5g氢氧化锂水溶液和0.005％的上述改性石墨烯，在115℃皂化3小时后升温至200℃脱水，急冷至温度145℃，然后剪切、均质和脱气，制得改性石墨烯基锂基润滑脂。
实施例5
将实施例1得到的改性石墨烯，加入1g含有0.005g硬脂酸表面改性偶联剂的溶剂，通过超声分乳化后在温度为60℃处理3h，过滤、干燥后制得改性石墨烯粉体；将95g润滑脂的基础油预热，然后加入2g 12-羟基硬脂酸，3g氢氧化锂水溶液和0.01％的上述改性石墨烯，在110℃皂化3小时后升温至205℃脱水，急冷至温度150℃，然后剪切、均质和脱气，制得石墨烯基锂基润滑脂。
实施例6
将实施例2得到的改性石墨烯，加入1g含有0.009g十六烷基三甲基溴化铵表面改性偶联剂的溶剂，通过超声分乳化后在温度为40℃处理5h，过滤、干燥后制得改性石墨烯粉体；将89g润滑脂的基础油预热，然后加入5g羟硬脂酸，6g硅酸水溶液和0.09％的上述改性石墨烯，在100℃皂化3小时后升温至210℃脱水，急冷至温度165℃，然后剪切、均质和脱气，制得石墨烯基硅酸润滑脂。
实施例7
将实施例3得到的改性石墨烯，加入1g含有0.008gγ-缩水甘油氧基丙基表面改性偶联剂的溶剂，通过超声分乳化后在温度为50℃处理4h，过滤、干燥后制得改性石墨烯粉体；将92g润滑脂的基础油预热，然后加入4g12-羟基硬脂酸，4g氢氧化钙水溶液和0.08％的上述改性石墨烯，在110℃皂化3小时后升温至210℃脱水，急冷至温度150℃，然后剪切、均质和脱气，制得石墨烯基钙基润滑脂。
实施例8
将实施例1得到的改性石墨烯，加入1g含有0.007gγ-缩水甘油氧基丙基表面改性偶联剂的溶剂，通过超声分乳化后在温度为50℃处理4h，过滤、干燥后制得改性石墨烯粉体；将91g润滑脂的基础油预热，然后加入4g硬脂酸，5g氢氧化钠水溶液和0.08％的上述改性石墨烯，在110℃皂化3小时后升温至205℃脱水，急冷至温度145℃，然后剪切、均质和脱气，制得石墨烯基钠基润滑脂。
实施例9
将实施例3得到的改性石墨烯，加入1g含有0.007g十六烷基三甲基溴化铵表面改性偶联剂的溶剂，通过超声分乳化后在温度为40℃处理5h，过滤、干燥后制得改性石墨烯粉体；将90g润滑脂的基础油预热，然后加入4g 12-羟基硬脂酸，6g氢氧化钙水溶液和0.07％的上述改性石墨烯，在115℃皂化3小时后升温至200℃脱水，急冷至温度150℃，然后剪切、均质和脱气，制得石墨烯基钙基润滑脂。
实施例10
将实施例1得到的改性石墨烯，加入1g含有0.006g硬脂酸表面改性偶联剂的溶剂，通过超声分乳化后在温度为60℃处理3h，过滤、干燥后制得改性石墨烯粉体；将92g润滑脂的基础油预热，然后加入3g 12-羟基硬脂酸，5g氢氧化钙水溶液和0.07％的上述改性石墨烯，在108℃皂化3小时后升温至205℃脱水，急冷至温度160℃，然后剪切、均质和脱气，制得石墨烯基钙基润滑脂。
实施例11
将实施例1得到的改性石墨烯，加入1g含有0.006g油酸表面改性偶联剂的溶剂，通过超声分乳化后在温度为30℃处理6h，过滤、干燥后制得改性石墨烯粉体；将90g润滑脂的基础油预热，然后加入3g十二羟基硬脂酸甲醋，7g氢氧化锂水溶液和0.06％的上述改性石墨烯，在105℃皂化3小时后升温至205℃脱水，急冷至温度155℃，然后剪切、均质和脱气，制得石墨烯基锂基润滑脂。
性能测试
将实施例4～11制备得到的润滑脂进行相应的性能测试，其性能测试数据见下表1。
表1润滑脂性能测试结果
结果表明，本发明制备得到的添加改性石墨烯润滑脂具有极低的摩擦系数(摩擦系数小于0.1)，其中实施例10和实施例11的摩擦系数达到0.04，还有优良的散热性能(热传导系数大于2.5W/mK)，且防腐蚀性、氧化安定性、抗磨性、低温转矩的性能也都达到很好的效果，所述润滑脂将在工业机器人谐波减速器润滑方面有很大的发展前景。
Claims (10)
1.一种掺杂二氧化硅的改性石墨烯的制备方法，其特征在于，将过量石墨烯分散在水中，剧烈搅拌，得到均匀分散液；然后将正硅酸乙酯，十六烷基三甲基溴化铵加入到上述溶液中，搅拌10～50分钟后将混合物于150～250℃水热处理2～4小时，分离沉淀、洗净、干燥，制得掺杂二氧化硅的改性石墨烯。
2.权利要求1所述制备方法制备得到的掺杂二氧化硅的改性石墨烯。
3.权利要求2所述掺杂二氧化硅的改性石墨烯在制备抗磨剂或润滑脂中的应用。
4.一种添加改性石墨烯的机器人谐波减速器润滑脂组合物，其特征在于，包括润滑脂和占润滑脂重量0.001～0.2%的掺杂二氧化硅的改性石墨烯。
5.根据权利要求4所述的润滑脂组合物，其特征在于，所述润滑脂为锂基润滑脂、钙基润滑脂、钠基润滑脂、铝基润滑脂、极压润滑脂或硅酸润滑脂。
6.根据权利要求4所述的润滑脂组合物，其特征在于，所述掺杂二氧化硅的改性石墨烯还需经表面改性偶联剂改性。
7.根据权利要求6所述的润滑脂组合物，其特征在于，所述表面改性偶联剂为硬脂酸、油酸、γ-缩水甘油氧基丙基三甲氧基硅烷和十六烷基三甲基溴化铵中的一种或几种。
8.根据权利要求4所述的润滑脂组合物，其特征在于，所述表面改性偶联剂为掺杂二氧化硅的改性石墨烯的重量含量的0.1～2%。
9.权利要求4～8任一项所述添加改性石墨烯的机器人谐波减速器润滑脂组合物的制备方法，其特征在于，包括如下步骤：
S1.将掺杂二氧化硅的改性石墨烯添加到含有表面改性偶联剂改性的溶剂中，超声乳化后30℃～60℃处理3～6h，过滤、干燥后制得改性石墨烯粉体；
S2.将基础油预热，然后加入脂肪酸、碱以及0.001～0.2% S1制得改性石墨烯粉体，100～115℃皂化3小时后升温至200～210℃脱水，急冷至温度145～165℃，然后剪切、均质和脱气，制得润滑脂组合物；
其中，S1所述表面改性偶联剂的含量为掺杂二氧化硅的改性石墨烯的重量的0.1～2%。
10.根据权利要求9所述的制备方法，其特征在于，基础油用量为84～99%、脂肪酸为0.1～15%、碱为0.1～15%。
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