CN104017627B - A kind of preparation method of modified graphene oxide antiwear additive - Google Patents
A kind of preparation method of modified graphene oxide antiwear additive Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007866 anti-wear additive Substances 0.000 title 1
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 8
- 239000011575 calcium Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052796 boron Inorganic materials 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- GJJSDZSDOYNJSW-UHFFFAOYSA-N lanthanum(3+);borate Chemical compound [La+3].[O-]B([O-])[O-] GJJSDZSDOYNJSW-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- DOVLHZIEMGDZIW-UHFFFAOYSA-N [Cu+3].[O-]B([O-])[O-] Chemical compound [Cu+3].[O-]B([O-])[O-] DOVLHZIEMGDZIW-UHFFFAOYSA-N 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- VLCLHFYFMCKBRP-UHFFFAOYSA-N tricalcium;diborate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]B([O-])[O-].[O-]B([O-])[O-] VLCLHFYFMCKBRP-UHFFFAOYSA-N 0.000 claims description 3
- FVEBQRPNXIWEFI-UHFFFAOYSA-N B([O-])([O-])[O-].[Mo+4].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].[Mo+4].[Mo+4] Chemical compound B([O-])([O-])[O-].[Mo+4].B([O-])([O-])[O-].B([O-])([O-])[O-].B([O-])([O-])[O-].[Mo+4].[Mo+4] FVEBQRPNXIWEFI-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 239000000314 lubricant Substances 0.000 abstract description 11
- 239000007787 solid Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 230000001050 lubricating effect Effects 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000004519 grease Substances 0.000 description 16
- 238000005461 lubrication Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- -1 calcium borate-modified graphene Chemical class 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003879 lubricant additive Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Lubricants (AREA)
Abstract
本发明涉及一种改性氧化石墨烯抗磨剂的制备方法。本发明在三口烧瓶中加入氧化石墨烯和含硼、钼、钙、铜、稀土元素的化合物，在上述容器中加入有机溶剂搅拌加热，然后加入浓硫酸作为催化剂并反应，升温至溶剂的沸点蒸出溶剂，将产物放入真空干燥箱干燥，即得到改性氧化石墨烯抗磨剂。本发明克服了油质润滑剂和固体润滑剂，但它们都有成本高、使用条件较苛刻、更换麻烦、产生废物污染环境等问题。本发明利用氧化石墨烯超薄、超硬、超润滑、耐腐蚀、耐高温特性的特性，通过具有抗磨性能元素的表面改性，制备出性能优异的新型抗磨剂，该产品能够显著改善润滑剂的润滑性能，大幅减少机械运动表面的摩擦和磨损，具有节材和节能的功效。The invention relates to a preparation method of a modified graphene oxide antiwear agent. In the present invention, graphene oxide and compounds containing boron, molybdenum, calcium, copper, and rare earth elements are added to a three-necked flask, an organic solvent is added to the above-mentioned container for stirring and heating, then concentrated sulfuric acid is added as a catalyst and reacted, and the temperature is raised to the boiling point of the solvent to evaporate The solvent is removed, and the product is dried in a vacuum oven to obtain the modified graphene oxide antiwear agent. The invention overcomes the problems of oily lubricants and solid lubricants, but they all have the problems of high cost, harsh service conditions, troublesome replacement, waste generation and environmental pollution. The present invention utilizes the properties of graphene oxide to be ultra-thin, super-hard, super-lubricating, corrosion-resistant, and high-temperature-resistant, and through surface modification of elements with anti-wear properties, a novel anti-wear agent with excellent performance is prepared, which can significantly improve The lubricating performance of the lubricant can greatly reduce the friction and wear of the mechanical moving surface, and has the effect of saving material and energy.
Description
技术领域technical field
本发明属于润滑技术领域，特别涉及一种改性氧化石墨烯抗磨剂的制备方法。The invention belongs to the technical field of lubrication, in particular to a preparation method of a modified graphene oxide antiwear agent.
背景技术Background technique
据国际权威机构统计，金属材料磨损、腐蚀、疲劳三大损耗约占工业总产值的30％，摩擦磨损是普遍存在的自然现象。摩擦损失了世界约三分之一的一次能源，磨损是造成材料与设备破坏和失效的三种最主要的形式之一，润滑则是降低摩擦、减少或避免磨损的最有效技术。发展具有良好抗磨损性能、高承载能力、对磨损表面具有一定修复功能、对据国际权威机构统计，金属材料磨损、腐蚀、疲劳三大损耗约占工业总产值的30％，摩擦磨损是普遍存在的自然现象。摩擦损失了世界约三分之一的一次能源，磨损是造成材料与设备破坏和失效的三种最主要的形式之一，润滑则是降低摩擦、减少或避免磨损的最有效技术。发展具有良好抗磨损性能、高承载能力、对磨损表面具有一定修复功能、对环境无污染或少污染的润滑技术，是当代化学和材料科学及摩擦学的重要课题之一。According to the statistics of international authoritative organizations, the three major losses of metal material wear, corrosion and fatigue account for about 30% of the total industrial output value, and friction and wear are ubiquitous natural phenomena. Friction loses about one-third of the world's primary energy. Wear is one of the three main forms of damage and failure of materials and equipment. Lubrication is the most effective technology to reduce friction and reduce or avoid wear. The development has good wear resistance, high bearing capacity, and has a certain repair function on the worn surface. According to the statistics of international authoritative organizations, the three major losses of metal materials, wear, corrosion, and fatigue account for about 30% of the total industrial output value. Friction and wear are ubiquitous. of natural phenomena. Friction loses about one-third of the world's primary energy. Wear is one of the three main forms of damage and failure of materials and equipment. Lubrication is the most effective technology to reduce friction and reduce or avoid wear. It is one of the important topics of contemporary chemistry, material science and tribology to develop lubrication technology with good anti-wear performance, high load-carrying capacity, certain repair function on worn surface, and no or less pollution to the environment.
传统的极压润滑脂提高极压抗磨性能主要是含硫、氯和磷的有机化合物，尽管极压性能较好，但是硫、氯和磷化合物会产生腐蚀和环境污染问题。而广泛应用的二烷基二硫代磷酸锌(ZDDP)高效极压抗磨剂，现在已显得难于适应形势发展的需要。这是因为：(1)元素Zn会使某些合金轴承(主要指含银、铅部件)产生电化学腐蚀；(2)在高于160度的工况下会因急剧分解而丧失抗氧化和极压抗磨性能。因此，寻找能够克服ZDDP局限性的新型极压抗磨剂已成为润滑脂研发的热点。Traditional extreme pressure greases mainly contain organic compounds containing sulfur, chlorine and phosphorus to improve extreme pressure and anti-wear performance. Although the extreme pressure performance is good, sulfur, chlorine and phosphorus compounds will cause corrosion and environmental pollution problems. However, the widely used zinc dialkyldithiophosphate (ZDDP) high-efficiency extreme pressure antiwear agent has become difficult to meet the needs of the development of the situation. This is because: (1) element Zn will cause electrochemical corrosion of certain alloy bearings (mainly silver and lead-containing parts); (2) it will lose oxidation resistance and Extreme pressure and anti-wear properties. Therefore, searching for new extreme pressure antiwear agents that can overcome the limitations of ZDDP has become a hot spot in the research and development of lubricating greases.
在固体润滑剂中，长期以来，工业上用的润滑剂主要有两种：油质润滑剂和固体润滑剂，但它们都有成本高、使用条件较苛刻、更换麻烦、产生废物污染环境等问题。石墨作为固体润滑添加剂以其来源广、价格低、固体润滑效果好等特点，大量应用于工业生产已有上百年的历史。但是使用的超细石墨和二硫化钼粉末的颗粒尺寸为微米尺寸，缺点是混合均匀性差，利用率低，添加量高。Among solid lubricants, for a long time, there are mainly two types of lubricants used in industry: oily lubricants and solid lubricants, but they all have problems such as high cost, harsh service conditions, troublesome replacement, and waste pollution to the environment. . As a solid lubricant additive, graphite has been widely used in industrial production for hundreds of years due to its wide source, low price, and good solid lubricant effect. However, the particle size of ultrafine graphite and molybdenum disulfide powder used is micron size, and the disadvantages are poor mixing uniformity, low utilization rate and high addition amount.
石墨烯材料具有超大的形状比(平面大小/厚度比)，并保持了石墨的基本导电性质和优良的润滑、耐腐蚀、耐高温特性。研究表明，石墨烯是目前发现的材料当中强度最高的材料，具有内在的机械强度和类似石墨较低剪切力，并且具有层结构特点，所以是很好的固体润滑剂。Graphene material has a large shape ratio (plane size/thickness ratio), and maintains the basic conductive properties of graphite and excellent lubrication, corrosion resistance, and high temperature resistance. Studies have shown that graphene is the strongest material among the materials found so far. It has inherent mechanical strength and low shear force similar to graphite, and has layer structure characteristics, so it is a good solid lubricant.
发明内容Contents of the invention
本发明的目的在于克服上述缺陷，研制一种改性氧化石墨烯抗磨剂的制备方法。The object of the present invention is to overcome above-mentioned defect, develops a kind of preparation method of modified graphene oxide antiwear agent.
本发明的技术方案是：Technical scheme of the present invention is:
一种改性氧化石墨烯抗磨剂的制备方法，其主要技术特征在于在三口烧瓶中加入氧化石墨烯和含硼、钼、钙、铜、稀土元素的化合物，在上述容器中加入有机溶剂搅拌加热，然后加入浓硫酸作为催化剂并反应，升温至溶剂的沸点蒸出溶剂，将产物放入真空干燥箱干燥，即得到改性氧化石墨烯抗磨剂。A preparation method of a modified graphene oxide antiwear agent, the main technical feature of which is to add graphene oxide and compounds containing boron, molybdenum, calcium, copper, and rare earth elements into a three-necked flask, and add an organic solvent to the above container to stir Heating, then adding concentrated sulfuric acid as a catalyst and reacting, raising the temperature to the boiling point of the solvent to evaporate the solvent, and putting the product in a vacuum drying oven to dry to obtain the modified graphene oxide antiwear agent.
所述的氧化石墨烯是用Hummers方法制备的。The graphene oxide is prepared by the Hummers method.
所述的含硼、钼、钙、铜、稀土元素的化合物是指硼酸、硼酸镧、硼酸钼、硼酸钙，硼酸铜中的一种或者多种。The compounds containing boron, molybdenum, calcium, copper, and rare earth elements refer to one or more of boric acid, lanthanum borate, molybdenum borate, calcium borate, and copper borate.
所述的氧化石墨烯和含硼、钼、钙、铜、稀土元素的化合物的重量比为1∶0.5-3。The weight ratio of the graphene oxide to the compound containing boron, molybdenum, calcium, copper and rare earth elements is 1:0.5-3.
所述的有机溶剂为石油醚、水、乙醇，苯，正己烷，氯仿。Described organic solvent is sherwood oil, water, ethanol, benzene, n-hexane, chloroform.
所述浓硫酸催化剂的重量为反应物的0.1-0.5％。The weight of the concentrated sulfuric acid catalyst is 0.1-0.5% of the reactant.
所述的反应温度60-150℃，反应时间为2-8h。The reaction temperature is 60-150° C., and the reaction time is 2-8 hours.
所述的产物的真空干燥温度为20-80℃。The vacuum drying temperature of the product is 20-80°C.
本发明的优点和效果在于利用氧化石墨烯超薄、超硬、超润滑、耐腐蚀、耐高温特性的特性，利用氧化石墨烯表面丰富的羟基和羧基，通过化学方法用具有抗磨性能的元素化合物对其进行改性，通过具有抗磨性能元素的表面改性，制备出性能优异的新型抗磨剂，该产品能够显著改善润滑剂的润滑性能，大幅减少机械运动表面的摩擦和磨损，具有节材和节能的功效。The advantages and effects of the present invention are that utilizing graphene oxide's ultra-thin, ultra-hard, super-lubricating, corrosion-resistant, and high-temperature-resistant characteristics, utilizing the abundant hydroxyl and carboxyl groups on the surface of graphene oxide, chemically using elements with anti-wear properties Compounds modify it, and through the surface modification of elements with anti-wear performance, a new type of anti-wear agent with excellent performance is prepared. This product can significantly improve the lubricating performance of lubricants, and greatly reduce the friction and wear of mechanical moving surfaces. Material saving and energy saving effect.
本发明的其他具体优点和效果将在下面继续说明。Other specific advantages and effects of the present invention will be further explained below.
具体实施方式detailed description
实施例1：Example 1:
在250mL三口烧瓶中加入1.2g氧化石墨烯和3.6g硼酸，然后加入30ml石油醚搅拌加入0.024g浓硫酸，升温至60℃冷凝回流反应8h，然后蒸出溶剂。将产物放入80℃真空干燥箱干燥得灰白色固体，即为硼酸改性氧化石墨烯。按照0.05％比例添加入普通润滑脂中，磨斑直径从空白脂的0.96减小到0.38，磨损率减少了60％，摩擦系数从空白脂的0.106下降到0.04，摩擦系数减少了60％。Add 1.2g of graphene oxide and 3.6g of boric acid into a 250mL three-necked flask, then add 30ml of petroleum ether, stir and add 0.024g of concentrated sulfuric acid, heat up to 60°C for reflux for 8h, and then distill off the solvent. The product was dried in a vacuum oven at 80°C to obtain an off-white solid, which was boric acid-modified graphene oxide. Adding it to ordinary lubricating grease at a ratio of 0.05%, the wear spot diameter is reduced from 0.96 of the blank grease to 0.38, the wear rate is reduced by 60%, the friction coefficient is reduced from 0.106 of the blank grease to 0.04, and the friction coefficient is reduced by 60%.
氧化石墨烯是用Hummers方法制备的，属于采用现有技术制备，故省略具体制备方法。Graphene oxide is prepared by the Hummers method, which belongs to the prior art, so the specific preparation method is omitted.
实施例2：Example 2:
在250mL三口烧瓶中加入1g氧化石墨烯和0.5g硼酸钙，然后加入70ml正己烷搅拌加热至60℃加入0.005g滴浓硫酸，继续升温至150℃冷凝回流反应2h，然后蒸出溶剂。将产物放入20℃真空干燥箱干燥得灰白色固体，即为硼酸钙改性氧化石墨烯。按照0.5％比例添加入普通润滑脂中，磨斑直径从空白脂的0.96减小到0.20，磨损率减少了80％，摩擦系数从空白脂的0.106下降到0.02，摩擦系数减少了80％。Add 1g of graphene oxide and 0.5g of calcium borate into a 250mL three-neck flask, then add 70ml of n-hexane, stir and heat to 60°C, add 0.005g of concentrated sulfuric acid dropwise, continue to heat up to 150°C, condense and reflux for 2h, and then distill off the solvent. The product was dried in a vacuum oven at 20°C to obtain an off-white solid, which was calcium borate-modified graphene oxide. Adding 0.5% to ordinary grease, the wear spot diameter is reduced from 0.96 of blank grease to 0.20, the wear rate is reduced by 80%, the friction coefficient is reduced from 0.106 of blank grease to 0.02, and the friction coefficient is reduced by 80%.
实施例3：Example 3:
在250mL三口烧瓶中加入1g氧化石墨烯和1.5g硼酸镧然后加入50ml乙醇搅拌加热至80℃加入0.020g浓硫酸，继续升温至130℃冷凝回流反应5h，然后蒸出溶剂。将产物放入60℃真空干燥箱干燥得灰白色固体即为硼酸镧氧化石墨烯。按照0.1％比例添加入普通润滑脂中，磨斑直径从空白脂的0.96减小到0.28，磨损率减少70％左右，摩擦系数从空白脂的0.106下降到0.04，摩擦系数减少了60％左右。Add 1g of graphene oxide and 1.5g of lanthanum borate into a 250mL three-neck flask, then add 50ml of ethanol, stir and heat to 80°C, add 0.020g of concentrated sulfuric acid, continue to heat up to 130°C, condense and reflux for 5h, and then distill off the solvent. The product was dried in a vacuum oven at 60°C to obtain an off-white solid which was lanthanum borate graphene oxide. Adding it to ordinary lubricating grease at a ratio of 0.1%, the wear scar diameter is reduced from 0.96 of the blank grease to 0.28, the wear rate is reduced by about 70%, the friction coefficient is reduced from 0.106 of the blank grease to 0.04, and the friction coefficient is reduced by about 60%.
实施例4：Example 4:
在250mL三口烧瓶中加入1g氧化石墨烯和1.2g硼酸铜然后加入10ml乙醇搅拌加热至40℃加入0.023g浓硫酸，继续升温至120℃冷凝回流反应4h，然后蒸出溶剂。将产物放入40℃真空干燥箱干燥得灰白色固体，即为硼酸铜改性氧化石墨烯。按照0.08％比例添加入普通润滑脂中，磨斑直径从空白脂的0.96减小到0.28，磨损率下降为空白的70％，摩擦系数从空白脂的0.106下降到0.02，摩擦系数减少了80％。Add 1g of graphene oxide and 1.2g of copper borate into a 250mL three-neck flask, then add 10ml of ethanol, stir and heat to 40°C, add 0.023g of concentrated sulfuric acid, continue to heat up to 120°C, condense and reflux for 4h, and then distill off the solvent. The product was dried in a vacuum oven at 40°C to obtain an off-white solid, which was copper borate-modified graphene oxide. Adding 0.08% to ordinary grease, the wear scar diameter is reduced from 0.96 to 0.28 of the blank grease, the wear rate is reduced to 70% of the blank grease, and the friction coefficient is reduced from 0.106 to 0.02 of the blank grease, and the friction coefficient is reduced by 80%. .
应用本发明得到的改性氧化石墨烯抗磨剂，添加入润滑剂中的比例为0.05％-0.5％，磨损率相比较空白脂减少了50-100％，摩擦系数相比较空白脂减少了50-100％。Applying the modified graphene oxide anti-wear agent obtained in the present invention, the ratio added to the lubricant is 0.05%-0.5%, the wear rate is reduced by 50-100% compared with the blank grease, and the friction coefficient is reduced by 50% compared with the blank grease -100%.
查看实施例1-4，可以看出，将改性石墨烯加入普通润滑脂中通过四球摩擦磨损试验机来对其进行了四球摩擦磨损实验，实验的条件为：压力392N；转速1200r/min；时间3600s。Looking at Examples 1-4, it can be seen that the modified graphene is added into the common grease to carry out the four-ball friction and wear test by the four-ball friction and wear tester. The experimental conditions are: pressure 392N; rotating speed 1200r/min; Time 3600s.
结果显示，经过改性的氧化石墨烯具有显著地减少磨损，降低摩擦系数的功效。The results show that the modified graphene oxide has the effect of significantly reducing wear and reducing the coefficient of friction.
表1：添加剂与基础油在不同比例下的表征Table 1: Characterization of additives to base oil at different ratios
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| CN105112124B (en) * | 2015-08-14 | 2018-05-15 | 中航联合石墨烯技术有限公司 | A kind of lubricant compositions based on graphene or graphene oxide and its preparation method and application |
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| CN106221858B (en) * | 2016-07-07 | 2018-12-21 | 重庆德领科技有限公司 | A kind of polymolecularity and the modified graphene lubricating oil of high-affinity and preparation method thereof |
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